Author Topic: 2010 Reference and Translation Requests  (Read 4063 times)

java

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Re: July 2010 Reference Request Thread
« Reply #160 on: August 10, 2010, 01:58:28 PM »
Requested by no1uno




A one-step method for the .alpha.-arylation of camphor. Synthesis of (-)-cannabidiol and (-)-cannabidiol dimethyl ether
Vaillancourt,Valerie;Albizati,Kim
J. Org. Chem.
1992, Vol.57(13), pp.3627–3631
DOI: 10.1021/jo00039a022


Abstract
The syntheses of (-)-cannabidiol and (-)-cannibidiol dimethyl ether were accomplished via fragmentation of an appropriately substituted 9-bromocamphor derivative. A new method of a-arylation of 3,9-dibromocamphor was shown to provide a variety of a-arylated camphor derivatives in good yield.



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Benzoxocin and benzoxonin derivatives. Novel groups of terpenophenols with central nervous system activity
Houry,Schlomo;Mechoulam,Rapael
J. Med. Chem.
1974, Vol.17(3),  pp.287–293
DOI: 10.1021/jm00249a006




Abstract
Condensation of carvone with olivetol gave a mixture of the two C-5 isomers of 5,6-dihydro-7-hydroxy-2-isopropyl-5-methyl-9-pentyl-2,6-methano-2H-1-benzoxin-4-(3H)-one (2a and 3a) and their positional isomer 4. These ketones were reduced to their respective alcohols, 5a, 6a, and 7a, which were converted to the olefins 8a, 9a, 12 and 13. Compounds 2a and 3a were deoxygenated to 10 and 11a. The benzoxonin 15a was obtained from the condensation of olivetol with a-pinene. The 1,2-dimethylheptyl homologs (on C-9) of 2a, 3a, 5a, 6a, 8a, 9a, 11a, and 15a were also prepared. Several of these compounds produced CNS depression in rats at doses equal to or less than those required for the natural ?6- and ?1-tetrahydrocannibinols.
« Last Edit: August 10, 2010, 02:04:02 PM by java »
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java

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Re: July 2010 Reference Request Thread
« Reply #161 on: August 10, 2010, 06:56:04 PM »
Requested by no1uno





An Efficient and Practical System for the Catalytic Oxidation of Alcohols, Aldehydes, and ?,?-Unsaturated Carboxylic Acids
Grill,Joseph;Ogle,James;Miller,Stephen
J. Org. Chem.
2006, Vol.71(25), pp.9291–9296
DOI: 10.1021/jo0612574




Abstract
Upon exposure to commercial bleach (5% aqueous sodium hypochlorite), nickel(II) chloride or nickel(II) acetate is transformed quantitatively into an insoluble nickel species, nickel oxide hydroxide. This material consists of high surface area nanoparticles (ca. 4 nm) and is a useful heterogeneous catalyst for the oxidation of many organic compounds. The oxidation of primary alcohols to carboxylic acids, secondary alcohols to ketones, aldehydes to carboxylic acids, and ?,?-unsaturated carboxylic acids to epoxy acids is demonstrated using 2.5 mol % of nickel catalyst and commercial bleach as the terminal oxidant. We demonstrate the controlled and selective oxidation of several organic substrates using this system affording 70?95% isolated yields and 90?100% purity. In most cases, the oxidations can be performed without an organic solvent, making this approach attractive as a “greener” alternative to conventional oxidations.



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99. The synthesis of myristicin
Trikojus,V;White,D
J. Chem. Soc.
1949, Vol.78(V),  pp.436-439
DOI: 10.1039/JR9490000436


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.....this may be interesting as it deals with the synthesis of the myristicin....java





Synthesis of Myristicin
VICTOR M. TRIKOJUS &  D. E. WHITE
nature
1939, 144, 1016-1016
doi:10.1038/1441016b0


Abstract
ALTHOUGH it is now many years since myristicin was first isolated from the oils of nutmeg and mace, its synthesis has not previously been recorded. Its constitution was established by H. Thoms in 19031 as 3-methoxy-4 : 5-methylenedioxy-l-allylbenzene, a molecule suitably orientated for its use as the starting point in the successful syntheses of cotarnine by Salway2 and by Becker and Decker3.
« Last Edit: August 10, 2010, 07:04:13 PM by java »
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August 2010 Reference Request Thread
« Reply #162 on: August 10, 2010, 07:06:51 PM »
Again , try to keep the format with all the information including the doi, so the person helping you can do their work more easily....java
« Last Edit: September 13, 2010, 03:49:35 PM by java »
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Re: August 2010 Reference Request Thread
« Reply #163 on: August 11, 2010, 01:25:19 AM »
Requested by no1uno



The Synthesis of N-(3-Methoxybenzyl)-N-methyl-3-methoxy-4,5-methylene-dioxyphenethylamine
Surrey,Alexander
J. Am. Chem. Soc.
1948, Vol.70(9), pp.2887–2890
DOI: 10.1021/ja01189a016




Abstract
The synthesis of N-(3-Methoxybenzyl)-N-methyl-3-methoxy-4,5-methylene-dioxyphenethylamine (I) was undertaken in order to determine whether it was identical to a-fagarine, the antifibrillatory agent isolated from the plant Fagara Coco. In 1945, Deulofeu and corworkers proposed a structure for a-fagarine in which the positions of the methoxy and methylenedioxy groups in ring A of I were not fixed. Inasmuch as the proposed structure can be considered an opened 2-benzyltetrahydroisoquinoline, it seemed reasonable to suspect that the groups in Ring A would occupy the positions shown in I.


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A Synthesis of N-(3-Methoxybenzyl)-N-methyl-3-methoxy-4,5-methylenedioxyphenethylamine
Hamlin,K;Weston,Arthur
J. Am. Chem. Soc.
1949, Vol.71(6), pp.2210–2212
DOI: 10.1021/ja01174a079




Abstract
The synthesis of N-(3-Methoxybenzyl)-N-methyl-3-methoxy-4,5-methylene-dioxyphenethylamine (I) was undertaken to determine its identity with a-fagarine, an alkaloid from the plant Fagara Coco. A comparison of physical data has shown I to be different from a-fagarine, thus confirming the results recently reported by Surrey, and by Redemann, Wisegarver and Icke.



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Antifibrillatory Agents. The Preparation of Some N-Benzyl-N-methylphenethylamines
Surrey,A;Mooradian,A;Cutler,R;Suter,Buck,J
J. Am. Chem. Soc.
1949, Vol.71(7), pp.2421–2422
DOI: 10.1021/ja01175a050




Abstract
A series of compounds having the structure I has been synthesized and found to have antifibrillatory action in varying degree.



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CXXXV.—The synthesis of substances allied to cotarnine
Salway,Arthur
J. Chem. Soc., Trans.
1909, Vol.95,  pp.1204-1220
DOI: 10.1039/CT9099501204

« Last Edit: August 11, 2010, 03:23:49 AM by java »
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Re: August 2010 Reference Request Thread
« Reply #164 on: August 12, 2010, 12:38:15 PM »
Requested by no1uno




The Hofmann Rearrangement Using Household Bleach: Synthesis of 3-Nitroaniline
Monk,Keith;Mohan,Ram
J. Chem. Educ.
1999, Vol.76(12),  p.1717
DOI: 10.1021/ed076p1717



Abstract
The Hofmann rearrangement is an important example of a rearrangement reaction that is discussed in most sophomore organic chemistry texts. Yet very few examples of this reaction can be found in lab texts. We have developed a simple experiment that involves the Hofmann rearrangement of 3-nitrobenzamide to give 3-nitroaniline using household bleach. The synthesis of 3-nitrobenzamide by nitration of benzamide and the subsequent Hofmann rearrangement can be carried out in two-and-a-half hours, making this a new and simple two-step reaction sequence for the organic laboratory.



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CCCCIII.—The Reimer–Tiemann reaction with m-bromo- and m-iodo-phenol
Hodgson,Herbert;Jenkinson,Thomas
J. Chem. Soc.
1927 pp.3041-3044
DOI: 10.1039/JR9270003041



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CCXII. A synthesis of safrole and o-safrole
Perkin,William;Trikojus,Victor
J. Chem. Soc.
1927 pp.1663-1666
DOI: 10.1039/JR9270001663



------------------------------

And this one ain't on PBS so a decent synthesis route would be great (preferably one NOT starting from dimethoxyethane,  the first step produces the D-Mannitol Acetonide):



Stereoselective and efficient synthesis of (S)-Pregabalin from d-Mannitol
Izquierdo,Sandra;Anguilera,Jordi;Buschmann,Helmut;Garcia,Monica;Torrens,Antoni;Ortuna,Rosa
Tetrahedron: Asymmetry
2008, Vol.19(6),  pp.651-653
doi:10.1016/j.tetasy.2008.03.005




Abstract
A straightforward synthesis of (S)-pregabalin in 28% overall yield starting from d-mannitol acetonide, as a primary source of chirality, is presented. The process is suitable for large-scale synthesis and involves simple and high-yielding chemical transformations as well as low-cost commercially available reagents.




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Enantiomerically Pure Synthesis of ?-Substituted ?-Butyrolactones: A Key Intermediate to Concise Synthesis of Pregabalin
Ok,Taedong;Jeon,Aram;Lee,Joohee;Lim,Jung;Hong,Chang;Lee,Hee-Seung
J. Org. Chem.
2007, Vol.72(19), pp.7390–7393
DOI: 10.1021/jo0709605




Abstract
Chiral ?-substituted ?-butyrolactones are known to be important intermediates for many biologically active compounds such as ?-aminobutyric acid (GABA) derivatives and lignans. We have developed a general, convenient, and scalable synthetic method for enantiomerically pure ?-substituted ?-butyrolactones, with either configuration, via nucleophilic cyclopropane ring opening of (1S,5R)- or (1R,5S)-bicyclic lactone followed by decarbethoxylation. The utility of our method was demonstrated by streamlined synthesis of pregabalin ((S)-3-isobutyl-?-aminobutyric acid), an anticonvulsant drug for the treatment of peripheral neuropathic pain.
« Last Edit: August 12, 2010, 01:00:02 PM by java »
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Re: August 2010 Reference Request Thread
« Reply #165 on: August 13, 2010, 10:35:54 AM »
Requested by Goldmember




The decomposition of daiacl peroxide—IV : Baeyer-Villiger reaction of optically active 3-methyl-4-phenyl-2-butanone
T. Kashiwagi, K. Fujimori, S. Kozuka and S. Oae,
Tetrahedron
1970, Volume 26, Issue 15, Pages 3647-3651
DOI:10.1016/S0040-4020(01)92942-4

« Last Edit: August 13, 2010, 10:38:55 AM by java »
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Re: August 2010 Reference Request Thread
« Reply #166 on: August 13, 2010, 10:50:24 AM »
Requested by no1uno

".......Has anyone seen a procedure for the preparation of hexachloroacetone (from the pentachloride preferably)... Alternatively, "


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Perhaloketones—XVII : Hexabromoacetone and the bromochloroperhaloacetones
Gilbert,E
Tetrahedron
1969, Vol.25(8), pp.1801-1806
doi:10.1016/S0040-4020(01)82752-6




Abstract
Hexabromoacetone, and all eight possible bromochloroperhaloacetones, have been prepared by the bromination of acetone, and of the corresponding chloroacetones, respectively, in acetic acid in the presence of sodium acetate. Several of these have also been made by treatment of fluorochloroperhaloacetones with aluminium bromide, but hexachloroacetone with aluminum bromide gave mixtures. The ketones were converted to the corresponding amides.



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Perhalo Ketones. IV. The Reaction of Perhaloacetones with Phosphorus Pentachloride
Farah,Basil;Gilbert,Everett
J. Org. Chem.
1965, Vol.30(4), pp.1241–1242
DOI: 10.1021/jo01015a502




Abstract
The perhalofluorochloroacetones are not readily susceptible to attack by reagents that normally lead to the replacement of carbonyl oxygen. This inertness is in marked contrast with their considerable reactivity towards nucleophiles and other polar funtions.



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A Critical Examination of the Preparation of Polychlorinated Acetones
Fohlisch,Baldur;Zinser,Hartmut
Org. Prep. & Proc. Int.
2004, Vol.36(6), pp.549-572
DOI: 10.1080/00304940409355973


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Halogenation
Pierce,Ogden;McBee,Earl
Ind. Eng. Chem.
1953, Vol.45(9), pp.1969–1975
DOI: 10.1021/ie50525a032




Abstract
Commercial production of chlorine and chlorinated organic compounds is still at a relatively high level but some decreases are evident especially in the area of insecticides and aromatics. In the field of chlorination research, the emphasis is still on improvements in techniques and processes especially in the categories of benzene hexachloride and of monomers and polymers. Fluorination research during the past year has been devoted primarily to hydrocarbons and olefins. The polymerization of chlorotrifluoroethylene has been studied quite extensively and a number of new polymers are described. The area of bromination is again concerned primarily with aliphatic and aromatic hydrocarbons. Several interesting investigations of the use of N-bromoamides and imides as brominating agents are described. Iodination still remains the least explored area of halogenation with only a few diversified investigations reported.
« Last Edit: August 13, 2010, 11:06:14 AM by java »
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Re: August 2010 Reference Request Thread
« Reply #167 on: August 15, 2010, 01:56:08 AM »
Reference by no1uno





Amino-Alcohols. IX. Biologic Assay of Propadrin and Ephedrine
Githens,Thomas
J. American Pharmaceutical Assoc.
1933, Vol.22(5),  pp.391-399
DOI: 10.1002/jps.3080220505




Abstract
The physiologic assay of phenylpropanolamine (propadrin) and phenylpropanolmethylamine (ephedrine) is a problem which still awaits completely satisfactory solution. Although the quantitative action of ephedrine has been elucidated fairly thoroughly, and it is known to act on most, if not all, of the structures innervated by the autonomic system, none of these actions lend themselves to accurate quantitative analysis. Its action on each of these structures differ so widely, quantitatively at least, from one animal to another and all are so markedly influenced by slight experimental differences which are not readily analyzed, that is is not possible to obtain quantitative determinations by comparing the action on one animal directly with that on another.



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Halogenation with Copper(II). II. Unsaturated Ketones
Kosower,Edward;Wu,G
J. Org. Chem.
1963, Vol.28(3),  pp.633–638
DOI: 10.1021/jo01038a008





Abstract
The halogenation procedure previously described was applied to a number of unsaturated ketones. 2-Cyclohexenone and 3-methyl-2-cyclohexenone gave phenol and m-cresol, respectively. Isophorone yielded 3-chloro-methyl-5,5-dimethyl-2-cyclohexenone and 6-chloro-3,5,5-trimethyl-2-cyclohexenone in about equal quantities along with a lesser quantity of some phenols. Mesityl oxide and isomesityl oxide form mixtures (in different proportions) of almost every possible monochlorinated product. Methyl vinyl ketone leads to 3-chloro-3-buten-2-one. The mechanisms for the halogenation reactions are discussed.




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8. Degradation of quaternary ammonium salts. Part V. Molecular rearrangement in related sulphur compounds
Thomson,Thomas;Stevens,Thomas
J. Chem. Soc.
1932 pp.69-73
DOI:  10.1039/JR9320000069




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Nucleophilic Displacement via Frontal Attack. The Stereochemistry of the Stevens Rearrangement
Brewster,James;Kline,Milton
J. Am. Chem. Soc.
1952, Vol.74(20), pp.5179–5182
DOI: 10.1021/ja01140a058




Abstract
The relation of the Stevens rearrangement to the amine replacement and alkylide-forming reactions of quaternary ammonium salts is discussed. d-a-Dimethylamino-B-phenylbutyrophenone, prepared by the Stevens rearrangement of the phenacyl bromide derivative of l-N,N-dimethyl-a-phenylethylamine, has been degraded to l-B-methylhydrocinnamic acid via Beckmann rearrangement of the oxime of the ketone formed by reductive deamination of the rearrangement product. The previously established configurational relation of l-N,N-dimethyl-a-phenylethylamine to l-B-methylhydrocinnamic acid shows that the a-phenylethyl group retains its original configuration during its intramolecular migration from nitrogen to carbon. The rearrangement occurs with little racemization; racemic forms of several of the degradation products are, however, concentrated by recrystallization. These findings lend strong support to the concept that nucleophilic displacement can occur by frontal as well as by lateral and rearward attack.
« Last Edit: August 15, 2010, 02:05:49 AM by java »
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Re: August 2010 Reference Request Thread
« Reply #168 on: August 15, 2010, 08:36:23 PM »
Requested by no1uno

" - the alkylphosphate esters should give P2O5 on pyrolysis, which means at last a decent route to P2O5..."




Alkyl Esters of Phosphoric Acid
Hochwalt,Carroll;Lum,J;Malowan,J;Dyer,C
Ind. Eng. Chem.
1942, Vol.34(1),  pp.20–25
DOI: 10.1021/ie50385a005




Abstract
The properties and applications of alkyl esters of phosphoric acid are discussed. From a commercial standpoint the esters of greatest interest are mixtures of monalkyl and dialkyl hydrogen phosphates. In these acid esters hydrogen is replaced by various basic groups including sodium, potassium, ammonia, and amines. Data are presented on such physical properties as solubility, freezing point. specific gravity, viscosity, and conductance of solutions. Chemical properties include stability to hydrolysis and corrosiveness to metals.
    The outstanding property of mixed lower alkyl phosphates is their high solubility in water. Their water solutions exhibit low freezing points, good humectancy, high conductivity, and good stability. Furthermore, they are not particularly corrosive.
The properties of concentrated water solutions of several of the alkyl phosphates are of advantage for certain industrial applications. Several esters are antistatic agents in the spinning of textile fibers. Ammonium alkyl phosphates are useful in flameproofing cloth and paper. The possess an advantage over inorganic phosphates as flameproofing agents in that they can be exposed to lower relative humidities wihtout crystallization. Other possible applications for the alkyl phosphates are indicated.




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Manufacture of Phosphoric Acid by the Volatilization Process: Some Technical Problems
Waggaman,Wm
Ind. Eng. Chem.
1942,  Vol.16(2) 1924 pp.176–179
DOI: 10.1021/ie50170a036




Abstract
The production of phosphoric acid by the volitization method has distinct advantages over the sulfuric acid method - (1) low-grade phosphates can be used, (2) costly filtration and evaporation are obviated by using the Cottrell method of precipitation, and (3) the cost of thermal energy required should be less than the cost of chemcial reagents necessary to affect the same results.
   The fuel furnace has been shown to cause volatization as efficient as the electric furnace, although radiation and heat losses are considerably less in the electric smelting. Such losses, however, can be considerably reduced.
   The question of what temperature is best adapted for the volatization, especially in the fuel furnace, is still only partially answered, since it is dependent upon other factors, such as the lime silica ratio in the charge, the fineness of division and intimate contact of the reacting materials, the amount of reducing agent present, the time factor, and the type of furnace used. The first of these factors is equally important in both electrical and fuel smelting.
    Another problem of commercial importance studied at this laboratory is the determination of the proper P2O5 content fo the residual slag for the most economic operation. There are a number of others which also offer fields for valuable research.



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Synthesis of Mono- and Dialkylphosphates by the Reactions of Hydroxycompounds with Phosphorus pentoxide the Phosphorus Pentoxide under Microwave Irradiation
Elias,Abdelhamid;Didi,M;Villemin,Didier;Seaoune,T;Outtas,S
Phosphorus, Sulfur, and Silicon and the Related Elements
Vol.179(12) 2004 pp.2599-2607
DOI: 10.1080/10426500490494705




Abstract
The reactions of phosphorus pentoxide with two alcohols and one phenol were performed in different conditions under microwave irradiation. The products (alkylphosphates and dialkylphosphates) were identical to those formed by classic heating and were obtained with better yields. The speed of the reaction was increased by a factor from 100 to 400C.

Keywords:Alkylphosphates;dialkylphosphate;microwave irradiation;solvent free




http://ifile.it/k8wvaec/phosphoric%20files.zip   this has all three files....i wasn't able to upload the first file so it's here in the zip
« Last Edit: August 16, 2010, 12:04:51 AM by java »
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Re: August 2010 Reference Request Thread
« Reply #169 on: August 17, 2010, 03:15:21 AM »
Requested by no1uno




The Interactions of Aqueous Solutions of Chlorine with Citric Acid. A Source of Mutagens. (A Preliminary Report)
Streicher,Robert;Zimmer,Hans;Bercz,J;Coleman,W
Analytical Letters
1986, Vol.19(5),  pp.681-696
DOI: 10.1080/00032718608064529



Abstract
Citric acid, an additive to an important acrylamide based polymeric flocculant, was found to react with an aqueous solution of chlorine to give several chlorinated propanones, di- and trichloroacetic acid, chloroform, and a number of as yet unidentified chlorine containing compounds. Formation of these alledged carcinogens and mutagens also takes place by treating diluted aqueous solutions of frozen orange juice concentrate with such chlorine solutions. The formation and ratios of the detected chlorinated compounds is pH-dependent. A tentative scheme which could account for these findings is presented.


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The Intehaction of Aqueous Solutions of Chlorine with Malic Acid, Tartaric Acid, and Various Fruit Juices: A Source of Mutagens
Chang,Tak-Lung;Streicher,Robert;Zimmer,Hans;Munch,J
Analytical Letters
1988, Vol.21(11), pp.2049-2067
DOI: 10.1080/00032718808059890



Abstract
The interactions of aqueous solutions of chlorine with some fruit acids (citric acid, DL-malic acid, arid L-tartaric acid) at different pH values were studied. Diethyl ether extraction followed by GC/MS analysis indicated that a number of mutagens (certain chlorinated propanones and chloral hydrate) are present as major products in some of these samples. A number of fruit juices (orange, grape, apple, pineapple, and grapefruit) were also treated with aqueous solutions of chlorine at their pH values. The products were analyzed by GC/MS. The same mutagens that were formed by the pure acids (citric acid and DL-malic acid) were identified as major products in ether extracts of these samples. Another mutagen, dichloroacetonitrile, was also identified as a minor product in some of these juice samples. All of the major products observed in the chlorination of all five fruit juices are potentially derived from reactions of aqueous solutions of chlorine with citric or malic acid and with trace amounts of acetaldehyde and acetone in the juices. The minor product, dichloroacetonitrile, is likely derived from the chlorination of certain amino acids in the fruit juices.

Keywords:DL-malic Acid;L-tartaric Acid;Mutagens;Chlorinated Propanones;Orange;Apple;Pineapple; Grapefruit;Dichloroacetonitrile;Chlorinated Acetic Acids; Chloroform;Chlorination;Amino Acids;Aspartic Acid;Trichloroacetaldehyde; Chloral Hydrate


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Chloroform and chlorophenol production by decarboxylation of natural acids during aqueous chlorination
Larson,Richard;Rockwell,Arlene
Environ. Sci. Technol.
1979, 13 (3), pp 325–329
DOI: 10.1021/es60151a014



Abstract
Naturally occurring carboxylic acids of several structural types reacted in dilute solution with aqueous hypochlorite to afford decarboxylation products. Incorporation of chlorine into the residual organic molecule occurred. Citric acid was efficiently converted to chloroform at pH.7. by a pathway probably involving 3-ketoglutaric acid as an intermediate; in acidic or alkaline solution, yields of CHCl3 were lower. Several other enolizable keto acids (including all three isomers of resorcylic acid) were likewise precursors of CHCl3; yields varied widely. Two substituted benzoic acids common to natural waters, p-hydroxybenzoic acid and vanillic acid were decarboxylated by hypochlorite with the production of chlorophenols



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Synthesis of 3-Methyl Isoquinolines*
Govindachari,T;Pai,B
J. Org. Chem.
1953, Vol.18(10),  pp.1253-1262
DOI: 10.1021/jo50016a004




Abstract
This paper is concerned with a study of the limitations and usefulness of a novel method developed by Bruckner and co-workers (1) for the synthesis of 3-methyl isoquinolines. Bruckner and co-workers have applied the method only to propenylbenzenes derived safrole and eugenol. The scheme of work in the present study is shown in Chart I. In the group of compounds employed, poor yields were obtained in the conversion of allylphenols to propenylphenols from which, in turn, pseudonitrosites were formed only in low yields. The study was therefore conducted with the O-methyl ethers of the allylphenols, which could be transformed in high yield to propenylanisoles (V) by treatment with alkali.[/color]


* I don't know why, but when I searched for Claisen Rearrangement 2,5-dimethoxypropenylbenzene this was the result. Therefore I suspect this paper may in fact deal with the rearrangment of 1-methoxy-4-allyloxybenzene & if so, it is FUCKING important.
« Last Edit: August 17, 2010, 03:38:13 AM by java »
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Re: August 2010 Reference Request Thread
« Reply #170 on: August 17, 2010, 01:15:31 PM »
Requested by no1uno


"I don't know why, but this paper is cited as the literature procedure for the preparation of N-(Trifluoroacetyl)-4-bromo-2,5-dimethoxycathinone via F/C Acylation of 2,5-dimethoxybromobenzene (By Glennon, et al, 2004)... As it is the only reference I've seen for starting from the 4-substituted dimethoxybenzene (which would remove a massive yield killer) it is of some interest."



Synthesis of the C-glycoside fragment of Nogalamycin and some Nogalamycin Precursors
Bates,Mark;Sammes,Peter;Thomson,Gordon
J. Chem. Soc.Perkin Trans. 1
[/i]1988 pp.3037-3045[/i]
DOI: 10.1039/P19880003037



Abstract
A short, stereoselective method for generation of the fused C-glycoside unit of the anticancer agent nogalamycin is described; in particular, synthesis of the D,E,F ring system. The method utilises a total synthesis of the glycosidic unit from an aryl furyl alcohol. Initial studies are described for the preparation of highly substituted phthalides, useful for the further annulation of the D,E,F ring system to the rest of the nogalamycin skeleton.
« Last Edit: August 17, 2010, 01:20:55 PM by java »
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Re: August 2010 Reference Request Thread
« Reply #171 on: August 19, 2010, 12:36:12 AM »
Requested by no1uno


"Hmm, thought I'd add these - they deal with the preparation of calcium hypophosphite from phosphine (the calcium sulphate is removed by filtration), the CaCl2 would not affect the product from where I'm sitting..."




812. Kinetics of the reaction between phosphine and sodium hypochlorite in alkaline solution
Lawless,J;Searle,H
J. Chem. Soc.
1962 pp.4200-4205
DOI: 10.1039/JR9620004200


----------


Absorption of phosphine in aqueous solutions of sodium hypochlorite and sulphuric acid
Chandrasekaran,K;Sharma,M
Chemical Engineering Science
1977, Volume 32, Issue 3,  Pages 275-280
DOI: 10.1016/0009-2509(77)80205-4



Abstract
The kinetics of absorption of phosphine in aqueous solutions of sodium hypochlorite and sulphuric acid was studied in a stirred cell and a stirred contactor. The reaction of phosphine with aqueous solutions of sodium hypochlorite was found to first order with respect to phosphine and hypochlorite. The effect of pH on the second order rate constant was also investigated. The value of the second order rate constant was found to vary from 230 to 77,000 1./g mole sec at 28°C in the pH range of 12.95-9.40.

The reaction of phosphene with aqueous solutions of sulphuric acid, in the range of concentrations of 80 to 92% by weight, was also found to be first order with respect to phosphine. The value of the pseudo first order rate constant was found to be in the range of 3 × 106?4 × 10' sec?1 at 28°C. Copper sulphate was found to be an effective catalyst in sulphuric acid solutions.
« Last Edit: August 19, 2010, 12:41:40 AM by java »
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Re: August 2010 Reference Request Thread
« Reply #172 on: August 19, 2010, 11:53:26 PM »
Requested by no1uno

"Working my way through an old reference request thread @SM and found a paper by Wurtz (requested by Sauron), which details the preparation of SOCl2 (aka Thionyl Chloride) from Sulfur and Dichlorine Monoxide (ie. S + Cl2O ==> SOCl2). I thought I'd have a quick look and see - I believe at least one or more of these papers has more detail on the process:"




Practical Synthesis of Dichlorine Monoxide
Hain,John;McGee,Henry
Ind. Eng. Chem. Prod. Res. Dev.
1983, Vol.23(3), pp.490–491
DOI: 10.1021/i300015a033




Abstract
A continuous reaction scheme and apparatus were designed to synthesize Cl2O for use in the generation of O2(1,Delta) from H2O2 for subsequent use in pumping the I atom laser at 1.315 um. Chlorine was reacted with anhydrous Na2CO3 in a fixed or fluidized bed reactor at 180C. The product gases were collected in CCl4 or in KI solution and analyzed in iodometric titration technique. Cl2 conversion was 89%.


-------------------



The Chemistry of Chlorine Monoxide (Dichlorine Monoxide)
Renard,J;Bolker,H
Chem. Rev.
1976, Vol.76(4), 487–508
DOI: 10.1021/cr60302a004


Contents

    I. Introduction
   II. Preparation
       A. Mercuric Oxide Method
       B. Sodium Carbonate and Allied Methods
       C. Preparation from Hypochlorous Acid Solutions
  III. Analysis
   IV. Physical Properties
       A. General
       B. Thermodynamic Properties
       C. Solubility
          1. Water
          2. Carbon Tetrachloride
    V. Structure and Stereochemistry
       A. Dipole Movement
       B. Ionization Potential-Mass Spectroscopy
       C. Molecular Genometry
       D. Photoelectron Spectroscopy
       E. Ultravoilet and Visible Spectroscopy
       F. Infrared Spectroscopy
       G. Raman Spectroscopy
       H. Microwave Spectroscopy
       I. The Cl-O Bond in Cl2O
   VI. Chemical Properties
       A. Photochemistry
          1. Photochemical Stability
          2. Photolysis of Gaseous Chlorine Monoxide
          3. Photolysis of ClCl2O in Carbon Tetrachloride Solution
          4. Photolysis of Matrix-Isolated Cl2O
       B. Thermochemistry
          1. Mechanism of Thermal Decomposition
          2. Explosive Decomposition
       C. Reactions with Inorganic Substances
          1. Hydrogen Atoms
          2. Other Atoms
          3. Alkaline and Alkali Earth Metals Hydroxides
          4. Alkaline Hydrogen Peroxide
          5. Nitrogen Oxides
          6. AsFCl5 and SbFCl5
          7. Metallic and Metalloidic Halides
          8. Fluorine
          9. Miscellaneous
       D. Reactions with Organic Compounds
          1. Saturated Compounds
          2. Unsaturated Compounds
          3. Phenols and Aryl Ethers
          4. Miscellaneous
  VII. Addendum
 VIII. References



-----------------




Dichlorine Monoxide: A Powerful and Selective Chlorinating Agent
Marsh,F;Farnham,W;Sam,D;Smart,B
J. Am. Chem. Soc.
Vol.104(17) 1982 pp.4680–4682
DOI: 10.1021/ja00381a032




Abstract
Dichlorine monoxide (Cl2O) has long been known and has been the subject of some modern mechanistic and physical studies, but it has not been shown to be a useful reagent in synthetic chemistry. We have found that Cl2O is a powerful and selective reagent for either side-chain or ring-chlorination of deactivated aromatic substrates, and it gives excellent yields under mild conditions fail or require harsh conditions.


----------------



Syntheses of Oxide Halides
Dehnicke,Dr.K
Ang. Chem. Int. Ed.
1965, Vol.4(1),  pp.22-29
DOI: 10.1002/anie.196500221




Abstract
Knowledge of the oxide halides has made significant advances in recent years as a result of new methods of preparation. Moreover, the systematic study of older methods has led to versatile syntheses which permit the preparation of many new oxide halides. A brief outline of the scope, limitations, and difficulties of the various processes is given together with a number of examples.
« Last Edit: August 20, 2010, 12:15:54 AM by java »
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Re: August 2010 Reference Request Thread
« Reply #173 on: August 20, 2010, 11:08:49 AM »
Requested by no1uno


"The first one is what grabbed my eye (that plus the stereospecific reduction of tropanone with alkoxides)... Looking further, how to make the KOEt/KOiPr, by the look of it, they are even easier to make than the NaOEt/NaOiPr... Noice..."



A Carbonyl Reduction by Potassium Hydroxide in Ethanol
Rubin,Martin
J. Am. Chem. Soc.
1944, Vol.66(12),  pp.2075–2076
DOI: 10.1021/ja01240a021




Abstract
The system ROH-ROM, particularly in the case where M is aluminium, is an efficient reagent, for the reduction of carbonyl compounds to the carbinols. Magnesium, tin, zirconium, sodium, zinc and calcium have been used in place of aluminium in this system. Potassium hydroxide in benzyl alcohol has been used to reduce soem aldehydes and potassium hydroxide in ethanol under reflux has been utilized for the reduction of substituted benzophenones and at 200-300o for high molecular weight aliphatic ketones. Under these conditions the potassium is predominantly in the form of the alkoxide.



------------------




Composition of Vapor and Liquid Phases in the Potassium Hydroxide + Methanol Reaction System at 25o
Platonov,Andrew;Kurzin,Alexander;Evdokimov,Andrey
J. Solution Chemistry
2010, Vol.39(3),  pp.335-342
DOI: 10.1007/s10953-010-9505-1




Abstract
The composition of the vapor and liquid phases of the KOH + CH3OH system has been studied by the gas chromatography (GC) method at 25?°C. It has been found that the methanol vapor concentration, and the quantity of potassium methoxide formed as a result of the acid–base reaction of potassium hydroxide with methanol, both depend on the KOH/CH3OH mole ratio. The maximum mass fraction of potassium methoxide that forms is 2.6% at the mole ratio 0.018.

Keywords:Potassium hydroxide;Methanol;Potassium methoxide;Vapor-liquid equilibrium



-------------------




Reaction Products of Ethyl Alcohol and Sodium Hydroxide
Williams,Dudley;Bost,R
J. Chem. Phys.
1939, Vol.4(4), pp.251-253
DOI: 10.1063/1.1749831




Abstract
A study has been made of the products formed when sodium hydroxide and ethyl alcohol react in the absence of water. Evidence has been found which indicates a reaction in which sodium ethylate and water are produced. Three types of tests have been made to determine the amount of water formed. The copper acetylide method, a volumetric method, and a method involving infrared absorption measurements all indicate a reaction which goes from 75 to 100 percent toward completion.



--------------------




Solubility of Potassium Carbonate in Methanol
Platonov,Andrew;Evdokimov,Andrey;Kurzin,Alexander;Maiyorova,Helen
J. Chem. Eng. Data,
2002, Vol.47(5),  pp.1175–1176
DOI: 10.1021/je020012v


Abstract
The solubility of potassium carbonate in methanol and the acid?base interaction of these compounds with each other have been considered. The reaction results in the formation of methoxide and hydrocarbonate of potassium. The reported values on the solubility of potassium carbonate differ essentially from the data described in the literature. The solubility of potassium hydrocarbonate in methanol has also been determined.
« Last Edit: August 20, 2010, 11:27:14 AM by java »
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Re: August 2010 Reference Request Thread
« Reply #174 on: August 20, 2010, 02:12:54 PM »
Requested by no1uno



The Chemistry of Phosphine
Fluck,Ekkehard
Topics in Current Chemistry
1973, Vol.35(1),  pp.1-64
DOI: 10.1007/BFb0051358  


Abstract
The present article is a revised and extended version of the work previously published by Fluck and Novobilsky: Fortschr. chem. Forsch. 13, 125 (1969). It is especially concerned with the many new physico-chemical investigations which have been carried out on phosphine. The literature has been covered to the end of 1971 and in some cases beyond this date.
Translated from the German by Dr. R. E. Dunmur
« Last Edit: August 20, 2010, 02:17:11 PM by java »
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Re: August 2010 Reference Request Thread
« Reply #175 on: August 20, 2010, 05:57:35 PM »
Requested by no1uno


""Shit, according to that last paper, phosphine burns in chlorine atmosphere to give PCl5... That could be handy......Has anyone got GC's preparation via a thermite-type reduction of AlP? A shitty, simple synthesis appeals"




The Chlorination of Metals in the Presence of a Donor Solvent
Osthoff,Robert;West,Robert
J. Am. Chem. Soc.
1954,Vol.76(18),  pp.4732–4734
DOI: 10.1021/ja01647a071





Abstract
A method for the low temperature chlorination of cobalt, nickel, manganese, zinc and chromium, in several donor solvents, is described. Several methods for the isolation of pure anhydrous metal halides or coordination compounds of the anhydrous halides have been established. It is shown that the halogenation of the metals in the presence of donor solvents is a rather general one; and that it must involve coordination of the solvent to the metals, for these reactions do not occur in non-polar solvents.


-----------



Preparation of Zinc Phosphide
Murali,K;Gopalam,B
J. Materials Science Letters
1986, Vol.5(10),  pp.989-990
DOI: 10.1007/BF01730258




Abstract
Zn3P2 has recently gained importance owing to its possible use in photovoltaic devices [1,2]. All previous investigations have been on materials synthesized by direct reaction of zinc and phosphorus. These material exhibit p-type conductivity which has been attributed to the presence of native defects (phosphorus interstitials).


-----------



On the Preparation of the Phosphides of Aluminum, Gallium and Indium
Addamiano,Arrigo
J. Am. Chem. Soc.
1960, Vol.82(7),  pp.1537–1540
DOI: 10.1021/ja01492a005




Abstract
The phosphides of aluminiumm, gallium and indium can be prepared by reaction between those metals and zinc phosphide, Zn3P2, in a neutral atmosphere (argon, hydrogen) at about 800-900o. The reaction proceeds according to the scheme:

 2Me + Zn3P2 ==> 2MeP + 3Zn (Me = Al, Ga, Zn){sic}

with formation of the phosphides of the third group elements and evolution of zinc vapors. X-ray and analytical data are given. The yield of the reaction is a maximum for AlP, while some metal is left unreacted in the preparation of GaP and InP.

« Last Edit: August 21, 2010, 03:26:34 AM by java »
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Re: August 2010 Reference Request Thread
« Reply #176 on: August 22, 2010, 04:31:35 AM »
Requested by no1uno


"I've never seen an "easy" route to dibromoethane and the first article seems to provide one, if so ethylenediamine is going to be a LOT easier to synthesize:"




Preparation of No-carrier-added [1-11C]Ethylene and [1-11C]1,2-Dibromoethane as New Labelling Agents
shah,F;Pike,V;Dowsett,K
Applied Radiation and Isotopes
1997, Vol.48(7),  pp.931-941
DOI: 10.1016/S0969-8043(97)00006-7




Abstract
A method is described for the preparation of NCA [1-11C]ethylene based on the passage of [1-11C]ethanol over heated (500°C) quartz glass in a stainless steel tube (in preference to dehydration by catalysis on ?-alumina or pyrolysis). The [1-11C]ethanol is prepared from cyclotron-produced NCA [11C]carbon dioxide by 11C-carboxylation of methylmagnesium bromide, freshly prepared in dibutyl ether, and reduction of the adduct with lithium aluminium hydride in diglyme. The use of involatile solvents avoids the formation of carrier ethylene and radioactive and stable diethyl ether by cracking processes over the heated catalyst. The preparation takes 21 min from the end of radionuclide production and has a radiochemical yield of 44%, decay-corrected from [11C]carbon dioxide. NCA [1-11C]ethylene is converted quantitatively into [1-11C]1,2-dibromoethane when collected in a solution of bromine in carbon tetrachloride. The NCA [1-11C]ethylene and [1-11C]1,2-dibromoethane may serve as new and useful labelling agents.



--------




The Preparation of Methylamine
Jones,Hilton;Wheatley,Ruth
J. Am. Chem. Soc.
1918, Vol.40(9),  pp.1411–1415
DOI: 10.1021/ja02242a007




Abstract
During research on the commercial synthesis of adrenalin in 1907-1908, one of us had occasson to require large quantities of methylamine. We could not buy and were therefore forced to make what we needed. We at that time tried out all the methods we could find described in the literature for the production of methylamine, and found that described by Brochet and Cambier was easily the best.



----------------




An Elementary Laboratory Experiment Involving the Hofmann Rearrangement. The Preparation of Methylamine Hydrochloride from Acetamide by means of Calcium Hypochlorite
Hauser,C;Renfrow,W
J. Chem. Educ.,
1937, Vol.14(11),  pp.542-543
DOI: 10.1021/ed014p542




Abstract
The well-known Hoffman reaction by which an amide, in the presence of of chlorine or bromine and an alkali, is converted into a primary amine with one less carbon atom, is of considerable interest in organic chemistry. The reaction may be used in the "going down series", and it serves as a laboratory method for the preparation of a primary aliphatic amine. The reaction is of interest also because it involves a molecular rearrangement.
« Last Edit: August 22, 2010, 04:38:14 AM by java »
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Re: August 2010 Reference Request Thread
« Reply #177 on: August 22, 2010, 02:34:19 PM »
Requested by no1uno


"Here are a couple more, I'd like to find a way to make use of the 2-methyl-4-chlorophenol that would be the hydrolysis product of the MCPA Herbicide that comes cheap as shit, in big drums, as the dimethylamine salt. The dimethylamine I have a use for, I'd like to get rid of the chlorine from the ring of the hydrolysis product as the 2-methyl-1,4-hydroquinone would be a great precursor to DOM,...."






Photochemical Behaviour of 4-Chloro-2-Methylphenoxyacetic Acid: Influence of pH and Irradiation Wavelength
Zertal,Abdennour;Sehili,Tahar;Boule,Pierre
J. Photochem. & Photobiol. A: Chemistry
2001, Vol.146(1),  pp.37-48
DOI: 10.1016/S1010-6030(01)00534-2



Abstract
The kinetics of phototransformation of MCPA is studied under various irradiation conditions. The photocatalytic transformation on TiO2 in aqueous suspension is almost specific and leads to 4-chloro-2-methylphenol (P7) as the main photoproduct. The same product is obtained when MCPA is irradiated on silica in the absence of water. The direct phototransformation is more complex: the reaction is not influenced by oxygen but it depends on the pH of the solution and on the irradiation wavelength. With the anionic form irradiated between 254 and 350 nm, photohydrolysis of C–Cl bond is almost quantitative (yield>86%). It leads to the hydroxylated photoproduct P2. With the molecular form the main product P5 results from a photochemical rearrangement of the molecule. With both forms, some other photoproducts are also identified and quantified, particularly methylhydroquinone (P1) and P7. 2-Methylphenol (P6) is only obtained with the anionic form as a minor product. However, irradiation of solutions in sunlight or with lamps emitting mainly at 365 nm (about 2 and 6% of the light is emitted at 334 and 313 nm, respectively) yields P7 as the main photoproduct. Its formation is self-accelerated. This wavelength effect is attributed to reactions induced by quinonic compounds formed as intermediates since the disappearance of MCPA is more efficient in presence of quinonic products. P7 is also the major photoproduct when phototransformation is induced by nitrite ions or Fe(III) perchlorate. Besides, it appears from Microtox® test that photoproducts formed at wavelength shorter than 350 nm are more toxic to the marine bacterium Vibrio fischeri than the initial compound.

Author Keywords:MCPA;Photolysis;Photocatalysis;Photorearrangement;Wavelength effect;Induced phototransformation; Toxicity



« Last Edit: August 22, 2010, 04:34:32 PM by java »
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Re: August 2010 Reference Request Thread
« Reply #178 on: August 22, 2010, 04:34:03 PM »
Requested by no1uno





Oxidation and Dechlorination of Chlorophenols in Dilute Aqueous Suspensions of Manganese Oxides: Reaction Products
Ukrainczyk,Ljerka;McBride,Murray
Environmental Toxicology & Chemistry
1993, Vol.12(11),  pp.2015-2022
DOI: 10.1002/etc.5620121107




Abstract
Some monomeric and dimeric oxidation products of para- and/or ortho-chlorinated phenols in dilute (1 mmol/L phenol), acidified, aqueous suspensions of manganese oxide (Na-buserite) were identified by MS, Fourier-transform IR spectroscopy and UV/visible spectroscopy. The para-chlorinated phenols (4-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol, 4-chloro-2-methylphenol) gave corresponding p-benzoquinones (benzoquinone, 2-chlorobenzoquinone, 2,6-dichlorobenzoquinone, 2-methylbenzoquinone) as the detectable water-soluble oxidation products. Dimeric products were present in the extracts obtained by washing the oxide with methylene chloride. Michael addition of phenolate to quinone seems to be the predominant mode of coupling. Chlorinated phenols without chlorine in the para-position (2-chlorophenol, 2,6-dichlorophenol) were more difficult to oxidize and afforded diphenoquinones as the only detectable water-soluble products. For all studied phenols, with the exception of 2,4,6-trichlorophenol, the amount of water-soluble products accounts only for a small fraction of oxidized phenol. The quinone and diphenoquinone products readily couple with phenols into humuslike materials.

Keywords:Chlorophenols;Oxidation products;Quinones;Dechlorination;Buserite



--------------

---------------




Efficient Oxidative Dechlorination and Aromatic Ring Cleavage of Chlorinated Phenols Catalyzed by Iron Sulfophthalocyanine
Sorokin,Alexander;Meunier,Bernard;Séris,Jean-Louis
Science
1995, Vol.268(5214),  pp.1163-1166
DOI: 10.1126/science.268.5214.1163




Abstract
An efficient method has been developed for the catalytic oxidation of pollutants that are not easily degraded. The products of the hydrogen peroxide (H2O2) oxidation of 2,4,6,-trichlorophenol (TCP) catalyzed by the iron complex 2,9,16,23-tetrasulfophthalocyanine (FePcS) were observed to be chloromaleic, chlorofumaric, maleic, and fumaric acids from dechlorination and aromatic cycle cleavage, as well as additional products that resulted from oxidative  coupling. Quantitative analysis of the TCP oxidation reaction  revealed that up to two chloride ions were released per TCP molecule. This chemical system, consisting of an environmentally safe oxidant (H2O2) and an easily accessible catalyst (FePcS), can perform several key steps in the oxidative  mineralization of TCP, a paradigm of recalcitrant pollutants
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Re: August 2010 Reference Request Thread
« Reply #179 on: August 23, 2010, 02:37:30 PM »
Requested by no1uno


"Both EPA & DHA ethanolamides are Anandamide analogues, the binding is 5-10 times lower @CB1 (respectively), but that aside, how hard is it to buy several liters of fish oil?"



Preparation of Omega-3 PUFA Concentrates from Fish Oils via Urea Complexation
Ratnayake,W;Matthews,D;Ackmann,R
]Lipid / Fett
1988, Vol.90(10), pp.381–386
DOI: 10.1002/lipi.19880901002




Abstract
The effect of weight ratio of urea to fatty acids and the urea-fatty acid adduct crystallization temperature on the enrichment of eicosapentaenoic acid from marine oil fatty acids was studied. The optimum ratio of urea to fatty acids was found to be 3 : 1 for laboratory scale preparations and the optimum temperature for the formation of urea-fatty acid adduct was 1°C. At very low temperatures (?12, ?18, ?35°C) the recovery efficiency for EPA was reduced. Using these optimum values, enrichment of EPA and other n-3 polyunsaturated fatty acids via urea complexation was carried out on a pilot plant scale in a variety of North Atlantic and North Pacific fist oils and a seal oil. Irrespective of hte type of starting oil, all the oils gave a concentrate with 69–85% total n-3 PUFA with an overall yield of 17–20%. Menhaden is clearly an ideal oil for preparation of EPA concentrate, as the starting oil usually has a higher proportion of EPA to DHA than most of the other commercial fish oils.


---------------

Purification Process for Cod Liver Oil Polyunsaturated Fatty Acids
Guil-Guerrero,J;Belarbi,El-Hassan
J. Am. Oil Chem. Soc.
2001, Vol.78(5),  pp.477-484
DOI: 10.1007/s11746-001-0289-9




Abstract
The polyunsaturated fatty acids (PUFA) eicosapentaenoic acid (EPA, 20?5n?3) and docosahexaenoic acid (DHA, 22?6n?3), which have several pharmaceutical properties, have been purified from cod liver oil. The process consisted of four main steps: (i) saponification of the oil, (ii) use of urea inclusion adducts method to obtain PUFA, (iii) PUFA methylation, and (iv) argentation silica gel column chromatography of the methylated PUFA. Argentation silica gel chromatography yielded highly pure DHA in the process (100% purity, 64% yiild). For EPA, the recovery in the combined process was 29.6%, and the final purity was 90.6%, owing to the simultaneous elution of other polyunsaturated fatty esters. The recovery in the urea inclusion method was strongly enhanced by application of orbital agitation during the crystallization process, in which EPA yield increased from 60–70% without agitation to 90–97% at 800 rpm; stearidonic acid (18?4n?3) yield ranged from 60–75% without agitation to 87–95% at 800 rpm, and DHA yield varied from 53–73% without agitation to 85–99% at 800 rpm

Keywords:Argentation silica gel column chromatography;cod liver oil;docosahexanoenoic acid;eicosapentaenoic acid;polyunsaturated fatty acids;urea inclusion adducts



--------------




Separation and Preparative Purification of Arachidonic Acid from Microbial Lipids by Urea Inclusion Reaction and HPLC  
Yuan,Chengling;Wang,Xiangquin;Yu,Zengliang
Prep. Biochem. & Biotech.
2007, Vol.37(2),  pp.149-159
DOI: 10.1080/10826060701199098




Abstract
Arachidonic acid (AA) was separated and purified from microbial lipids by the combined method of urea inclusion reaction and reversed-phase high performance liquid chromatography. At first, AA was concentrated from free fatty acids made from microbial lipids by a urea inclusion reaction. The optimum conditions were as follows: methanol was the suitable solvent, the ratio of free fatty acids to urea to methanol was 1:2:8 (wt/wt), and the temperature of the urea inclusion reaction was -10°C. The AA content was increased from 38% to 79%, and then AA was purified on a C18 preparative column (300 mmtimes30 mm I.D., dp=15 µm), using methanol-water (95:5, v/v) as the mobile phase, at a flow rate of 5 mL/min. The purity of AA after two steps purification reached 99%. This result indicates that the combined method of the urea inclusion reaction and reversed-phase high performance liquid chromatography is a promising technique for purification of AA.

Keywords:Arachidonic acid;Polyunsaturated fatty acids;Urea inclusion reaction;Reversed-phase high performance liquid chromatography;Separation;Purification
« Last Edit: August 23, 2010, 02:46:36 PM by java »
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