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?"



Semi-Preparative HPLC Fractionation of Consumer Fish Oil (Triacylglycerols)
Wojtusik,Mary;Brown,Phyllis;Turcotte,Joseph
J. Liquid Chromatography & Related Technologies
1988, Vol.11(9 & 10),  pp.2091-2107
DOI: 10.1080/01483918808069042



Abstract
A reversed-phase high performance liquid chromatographic method was developed for the semi-preparative fractionation of fish oil-derived triacylglycerols containing the esterified omega-3 fatty acids all-cis-5,8,11,14,17-eicosapentaenoic acid [EPA] and all-cis-4,7,10,13,17,20-docosahexaenoic acid [DHA]. Analytical separation conditions, such as mobile phase composition and flow rate could be directly applied to the semi-preparative mode, which was further optimized. Separation of triacylglycerol fractions was obtained in 15 minutes using flow rates of 3.0 ml/min with a mobile phase of acetone/acetonitrile (65:35, v/v). 250-mg samples of the fish oil were fractionated and multi-milligram quantities of triacylglycerols were separated, which were 65% enriched in esterified EPA and DHA; a production rate of 500 mg/hr of this enriched fraction was obtained.

Requested by no1uno


"Yeah, there is a bunch... There may be some gems amongst them, Synthetic Pages has the preparation of Tosyl Bromide from toluenesulfinic acid (orgsyn also has at least one preparation where the TsOH is reduced to the correspondent sulfinyl with Zn."




The Removal of Oxygen from Gas Streams: Applications in Catalysis and Gas Chromatography
McLlwrick,C;Phillips,C
J. Phys. E: Sci. Instrum.
1973, Vol.6(12),  pp.1208
DOI: 10.1088/0022-3735/6/12/034



Abstract
Manganese (11) oxide supported on Celite has been found to reduce the oxygen concentration in nitrogen streams to 1 part in 109.5, as measured by the resistance of a heated cobalt oxide filament. The supported manganese oxide has been used specifically to protect catalytic materials the properties of which are studied by using them as gas chromatographic columns. Its chromatographic and noncatalytic properties enable it where necessary to be packed directly into such columns.



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Preparation and Properties of Anhydrous Acetic Acid
Eichelberger,William;la Mer,Victor
J. Am. Chem. Soc.
1933, Vol.55(9),  pp.3633–3634
DOI: 10.1021/ja01336a023




Abstract
Cryoscopic and solubility investigations with acetic acid as solvent require the preparation of anhydrous material of high purity in large quantities. The melting point must be highly reproducible without entailing undue labor.



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Spectrophotometric Titration of Water in Acetic Acid
Bruckenstein,Stanley
Anal. Chem.
1959, Vol.31(11),  pp.1757–1760
DOI: 10.1021/ac60155a018




Abstract
A direct spectrophotometric titration of water in glacial acetic acid  based upon the sulfuric acid-catalyzed hydrolysis of acetic anhydride has been applied to the determination of water in the concentration range 0.009 to 1.7%. The relative merits of sulfuric and perchloric acids as catalysts and the mechanism of the catalysis are discussed.



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A Modified Preparation of Triacetyl Borate
Ritscher,James;Kowalski,Denise;McKeon,James
J. Chem. Educ.
1974, Vol.51 (10),  pp.688-68x
DOI: 10.1021/ed051p688




Abstract
This modified preparation is safer than previous, widely used methods.



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Silicon Tetrabenzoate[//u]
Lanning,J
J. Org. Chem.
1954, Vol.19(7),  1171–1173
DOI: 10.1021/jo01372a025




Abstract
The method for preparing silicon esters from silicon tetrachloride nad sodium salts of organic acids has been used by Schuyten, Weaver and Reid (1) to prepare silicon tetraacetate and by Lanning (2) to prepare silicon tetrapropionate.



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On Esters of p-Toluenesulfonic Acid
Tipson,R
J. Org. Chem.
1944]Vol.9(3),  pp.235–241
DOI: 10.1021/jo01185a005




Abstract
During the past few years the esters of p-toluenesulfonic acid have achieved considerable practical importance as alkylating agents. They are particularly useful for the alkylation of phenolic substances containing one or more tertiary nitrogen atoms, since they react preferentially with the phenolic hydroxyl group and effect very littel alkylation of the tertiary nitrogen atom.



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The Preparation of Sulfinic Acids
Truce,William;Murphy,Anna
Chem. Rev.
1951, Vol.48(1),  pp.69–124
DOI: 10.1021/cr60149a004




Contents

     I. Introduction
    II. Reduction of Sulfonyl Halides to Sulfinic Acids
   III. Sulfuinination of Organometallic Compoudns
    IV. Friedel-Crafts Sulination of an Aromatic Gorup
     V. Replacement of a Diazonium Salt Group
    VI. Basic Cleavage of Sulfones
   VII. Rearrangment of o-SUbsittuted Aromatic Sulfones and Related Types
  VIII. Miscallaneous Methods
    IX. References

Requested by no1uno


"And now some more on the Silanes:"


1012. Reactions of aluminium chloride with dimethylsiloxanes

Cordischi,D;Mele,A;Somogyi,A
J. Chem. Soc.
1964 pp.5281-5283
DOI: 10.1039/JR9640005281

Abstract



NB I'm interested to see what the product is, this is everyday silicon for gaskets, etc. The product of its reaction with AlCl3 may be quite interesting, especially if it gives Silicon chlorides, from which acetic/propionic/benzoic anhydrides are easily made. There is also the potential for a molten salt type-production of SiCl4, which would make acetic/propionic anhydride very easy to procure.

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Preparation of Disilicon Hexachloride

Quig,Joseph;Wilkinson,John

J. Am. Chem. Soc.
Vol.48(4) 1926 pp.902–906
DOI: 10.1021/ja01415a008

Abstract

In reviewing the methods that have been proposed for the preparation of disilicon hexachloride,1 that proposed by Martin seemed the best. Gatterman and Weinlig chlorinated metallic silicon at 300o and obtained a yield of 20% but this could not be duplicated in this laboratory.

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Review: The Use of Microwave Irradiation in the Processing of Glasses and Their Composites

Kharissova,Oxana;Kharisov,Boris;Ruiz-Valdez,Juan

Ind. Eng. Chem. Res.

Vol.49(4) 2010 pp.1457–1466
DOI: 10.1021/ie9014765

Abstract

The use of microwave (MW) radiation in glass processing is reviewed and compared to the usual processing techniques, such as glass melting, sintering, sealing, devitrification, coating, reinforcement with various substances, deposition by layers, etc. MW heating is known as a much-faster process (requiring minutes rather than hours), yielding good product quality, in comparison with the prolonged conventional thermal treatment of glass precursors.

NB The graphical abstract for the search result shows a flask in a microwave with a reflux column sticking out the top. As a lot of people have been trying to work out how to make this particular reaction vessel, I thought it might be of interest.

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Derivatives of Silicon Tetrachloride

Harold,Joseph

J. Am. Chem. Soc.
Vol.20(1) 1898 pp.13–29
DOI: 10.1021/ja02063a603

Abstract

The review of the reactions of these tetrachloride furnishes some interesting data from which inferences of importance may be drawn. There are, however, numerous problems still unsolved, and many reactions that yet demand study, before any broad comparison of the behaviours of these elements can be definately made, or any conclusion as to the influence of the atomic weight or metallic character on the reactivity of their tetrachlorides established. No general rule could be deduced from the data already collected, which would enable us by a logically drawn analogy, to predict their behaviours in certain uninvestigated reactions

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Direct Formation of Element Chlorides from the Corresponding Element Oxides through Microwave-Assisted Carbohydrochlorination Reactions

Nordschild,S;Auner,N

Chemistry A: Eur. Journal
Vol.14(12) 2008 pp.3694–3702
DOI: 10.1002/chem.200701670

Abstract

A series of technically and economically important element chlorides—such as SiCl4, BCl3, AlCl3, FeCl2, PCl3 and TiCl4—was synthesized through reactions between hydrogen chloride and the corresponding element oxides in the presence of different carbon sources with microwave assistance. This process route was optimized for demonstration purposes for tetrachlorosilane formation and successfully demonstrates the broad applicability of various silicon oxide-containing minerals and materials for carbohydrochlorination. The chlorination reaction occurs at lower temperatures than with conventional heating in a tubular oven, with substantially shorter reaction times and in better yields: quantitatively in the case of tetrachlorosilane, based on the silicon content of the starting material. The experimental procedure is very simple and provides basic information about the suitability of element compounds, especially element oxides, for carbohydrochlorination. According to the general reaction sequence element oxide?element?element chloride used in today's technology, this one-step carbohydrochlorination with hydrogen chloride is considerably more efficient, particularly in terms of energy input and reaction times, avoiding the isolation of the pure elements required for chlorination to give the element chlorides with use of the more corrosive and toxic chlorine gas.

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A Study of Several Reactions of Carbon Tetrachloride Synthesis

Fink,Colin;Bonilla,Charles

J. Phys. Chem.
Vol.37(9) 1933 pp.1135–1167
DOI: 10.1021/j150351a006

Abstract

The manufacture of carbon tetrachloride, mainly for use as a grease solvent or as a fire extinguisher, is a relatively important industry. In 1925 the value of the output had reached the million dollar mark. Owing to its advantageous properties, the demand for carbon tetrachloride would undoubtedly increase if its price could be decreased. A glance at current prices shows carbon tetrachloride at about 6 cents per pound in drums and chlorine at below 2 cents in tank cars. There would seem to be much advantage in in the discovery of a process of manufacture of carbon tetrachloride superior to that of the old carbon bisulfide chlorination process now in use.

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The Halides and Oxyhalides of Silicon.

Schumb,Walter

Chem. Rev.
Vol.31(3) 1942 pp.587–595
DOI: 10.1021/cr60100a004

Abstract

The preparation and some of the properties of the silicon halides, oxyhalides, and related compounds are briefly described, with special reference to the results of recent research in the field. A comparison is offered of the compounds of silicon with those of carbon and the elements in Group IV a; similarities and differences are pointed out. The possible application of the oxyhalides of silicon to the synthesis of silicon resins is suggested.

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

Reaction of Carboxylic Acids with Tetrachlorosilane
Voronkov,M;Vlasov,A;Belousova,L;Grigor'eva,O;Vlasova,N

Russ. J. Org. Chem.
Vol.46(3) 2010 pp.318-321
DOI: 10.1134/S1070428010030024



Abstract
Tetrachlorosilane reacted with carboxylic acids RCOOH (R = Me, Bu, t-Bu) to give the corresponding acid chlorides RCOCl in 75–95% yield. The reactions of SiCl4 with trichloroacetic and 2-fluorobenzoic acids (R = Cl3C, 2-FC6H4) occurred more difficultly, presumably for steric reasons, and the yields of the corresponding acid chlorides were 11 and 22%, respectively. Tetrachlorosilane failed to react with stearic acid under analogous conditions. Products of the reactions of SiCl4 with chloroacetic and benzoic acids RCOOH (R = ClCH2, Ph) were tetraacyloxysilanes Si(OCOR)4, and tetrakis(chloroacetoxy)silane was formed in almost quantitative yield. The reaction of SiCl4 with glutaric acid led to the formation of a rubber-like polymeric material with the composition C5H6Cl2O4Si. The effect of pKa values of carboxylic acids on the direction and mechanism of the examined reaction is discussed.



The utility of some of these "MIGHT" result in improvements in the field of @Home syntheses, which is all I'm trying to do, when the other silicon papers are in, I'll put a whole new topic up in References dealing with the use of SiCl4 to prepare anhydrides (IMHO it is the best route by far for home chemists).

Requested by no1uno




Bactericidal Properties of Monoethers of Dihydric Phenols. II. The Monoethers of Resorcinol
Klarmann,Emil;Gatyas,Louis;Shternov,Vladimir
J. Am. Chem. Soc.
1931, Vol.53(9), pp.3397–3407
DOI: 10.1021/ja01360a025




Abstract
During the past several years a considerable amount of work has been carried out dealing with the influence of substitution by alkyl and aryl groups upon the antiseptic properties of mono- and polyphenols. The continued interest in this field of research is due to the occurrence among the mono- and polyhydric phenol homologs of many compounds which combine a remarkable bactericidal potency with a low toxicity for the animal organism. With few exceptions the products in question carry the substituted groups attached to the carbon atoms of the nuclei, while only few data are available on phenol derivatives in which an alkyl or aryl group is attached to another substituting element



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Bactericidal Properties of Monoethers of Dihydric Phenols. II. The Monoethers of Hydroquinone
Klarmann,Emil;Gatyas,Louis;Shternov,Vladimir
J. Am. Chem. Soc.,
1932, Vol.54(1),  pp.298–305
DOI: 10.1021/ja01340a045




Abstract
It has been shown in the preceding communication (Part I of this series) that among the monoethers of resorcinol there are a number of compounds which show very considerable bactericidal potency as determined with B. typhosus and Staphylococcus aureus as test organisms. This bactericidal efficacy was found to depend particularly upon the length of the chain and the molecular weight of the substituted aliphatic or aromatic radical.



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Bactericidal Properties of Monoethers of Dihydric Phenols. II. The Monoethers of Pyrocatechol. Comparative Notes on the Three Series of Monoethers
Klarmann,Emil;Gates,Louis;Shternov,Vladimir
J. Am. Chem. Soc.
1932, Vol.54(3),  pp.1204–1211
DOI: 10.1021/ja01342a053




Abstract
The third and last group of monoethers studied in this series of investigations comprises the derivatives of pyrocatechol.

The antibacterial action of the parent compound pyrocatechol and of its methyl ether, guaicol has been studied by many investigators in the past. It is not intended to give a complete tabulation of these findings; the general conclusion may be drawn from them, that as a bactericidal agent, pyrocatechol is less effective than phenol, while guiacol shows practically the same potency as phenol. This is not true, however, of the inhibitory action. Thus according to Cooper and Mason the minimum concentration of pyrocatechol required to inhibit the growth of B. Coli at 37^o is almost one-half that of phenol, while in the case of B. fluorescens liquefaciens it is even less.


Note: author corrections are included
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[11C]-Dimethylamine as a Labeling Agent for PET Biomarkers
Jacobson,Orit;Mishani,Eyal
Applied Radiation & Isotopes
2008, Vol.66(2),  pp.188-193
DOI: 10.1016/j.apradiso.2007.08.012




Abstract
The dimethylamine functional group is a common component of the chemical structure of numerous drugs. The most commonly used synthetic route for carbon-11 labeled radiopharmaceuticals which contain the dimethylamine group is via C-11 methylation of the monomethyl amine precursors. Here we describe the radiosynthesis of [11C]dimethylamine (1) and its application in the direct labeling of several positron emission tomography (PET) imaging agents by-passing the preparation of the monomethyl amine precursors.

Requested by POSEIDON



Ammonium Salts of Aliphatic Carboxylic Acids
Saverio Zuffanti
J. Am. Chem. Soc.
1941, 63 (11), pp 3123–3124
DOI: 10.1021/ja01856a067

Requested by Quantum Dude




The Preparation of Substituted Diphenylethylamines and Diphenylethanolamines

Warren D. McPhee, Ernst S. Erickson Jr.
J. Am. Chem. Soc.
1946, 68 (4), pp 624–627
DOI: 10.1021/ja01208a028



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The Stability of Chelate Compounds. III. Exchange Reactions of Copper Chelate Compounds
R. B. Duffield, M. Calvin
J. Am. Chem. Soc.
1946, 68 (4), pp 557–561
DOI: 10.1021/ja01208a007



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Molecular Rearrangements. XI. The Deamination of 1,1-Diphenyl-2-amino-1-propanol
Ben M. Benjamin, Howard J. Schaeffer, Clair J. Collins
J. Am. Chem. Soc.
1957, 79 (23), pp 6160–6164
DOI: 10.1021/ja01580a015


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Schiff bases. Part II. Some ketimines prepared by decarboxylation of -amino-acids in the presence of ketones and their reaction and that of aldimines with phenyl isocyanate
A. F. Al-Sayyab, A. Lawson and J. O. Stevens
J. Chem. Soc. C,
1968, 411 - 415
DOI: 10.1039/J39680000411



Abstract
Some ketimines prepared by thermal decarboxylation of amino-acids in the presence of aromatic ketones, or directly from the corresponding amines, are described. In the case of -hydroxy-amines, ring closure takes place to give oxazolidines. Aromatic ketimines derived from o-hydroxyacetophenone react with phenyl isocyanate to give coumarin derivatives. Aldimines prepared from o-and p-hydroxy- and -methoxy-substituted benzaldehydes react with phenyl isocyanate to give s-triazine derivatives.



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Schiff bases. I. Thermal decarboxylation of alpha-amino-acids in the presence of ketone
A. F. Al-Sayyab, A. Lawson
J Chem Soc Perkin 1
1968;4:406-10



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The Absolute Configuration of threo-2-Amino-1,2-diphenylethanol. A Correction of the Literature
Gloria G. Lyle, William Lacroix
J. Org. Chem.
1963, 28 (4), pp 900–901
DOI: 10.1021/jo01039a003


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Evidence for an azomethine ylide intermediate in the carbonyl- assisted decarboxylation of sarcosine. Novel synthesis of dl-phenylephrine hydrochloride
George P. Rizzi
J. Org. Chem.
1970, 35 (6), pp 2069–2072
DOI: 10.1021/jo00831a098



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Novel synthesis of benzyl amines from benzaldehydes
George P. Rizzi
J. Org. Chem.
1971, 36 (12), pp 1710–1711
DOI: 10.1021/jo00811a036



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Pyridoxal-Catalyzed Decarboxylation of Amino Acids
G. D. Kalyankar, Esmond E. Snell
Biochemistry
1962, 1 (4), pp 594–600
DOI: 10.1021/bi00910a008

Requested by no1uno

"With regard to the second request, may I draw your attention to this article? They are using NORMAL bar magnets & shims to get H-NMR readings from that fucking unit by the looks of things (and the same is discussed in the first article). Hmmmmm, what couldn't we do with that? Knowing EXACTLY what is in the pot? Be nice wouldn't it?"



Design and construction of a dipolar Halbach array with a homogeneous field from identical bar magnets: NMR Mandhalas
Raich,H;Blumler,P
Mag. Res. Part B: Mag. Res. Eng.
2004, Vol.23B(1),  pp.16–25
DOI: 10.1002/cmr.b.20018




Abstract
Magnets of the Halbach layout are interesting for the use in mobile NMR/MRI devices. Therefore, the ideal Halbach magnet was iterated using identical bar magnets, which are positioned and oriented based on analytical equations. These configurations were simulated with two-dimensional finite-element methods. Performance factors were defined to related field strength with homogeneity and mass. A geometry of 16 magnets provided a good compromise between performance and special requirements for the desired use to store hyperpolarized xenon. The construction of such a magnet required the design of dedicated support frames and procedures to mount them. The field strength and homogeneity in the finished magnet were measured by a Hall probe and agreed well with the simulations. The calculation and construction are described in detail and together with the tabled field values for n magnets with n ? 80 may prove helpful for building similar devices, which were named NMR Mandhalas (Magnet Arrangements for Novel Discrete Halbach Layout).



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Small Magnets for Portable NMR Spectrometers
Danieli,Ernesto;Perlo,Juan;Blumich,Bernhard;Casanova,Federico
Angewandte Chem. Int. Ed.
2010, Vol.49(24),  pp.4133–4135
DOI: 10.1002/anie.201000221




Abstract
Downsizing: A pocket-size permanent magnet has been constructed that is suitable for measuring 1H-NMR spectra of samples in standard NMR tubes. The new shimming approach implemented to overcome the inherent inhomogeneity of permanent magnets opens the door to compact high-resolution NMR spectrometers for conventional samples.

Requested by Goldmember




Chlorination of tetrahydrofuran-2-carboxylic acid esters
R. A. Zhuk, A. é. Berzinya, V. N. Silinya, é. é. Liepin'sh and S. A. Giller
Chemistry of Heterocyclic Compounds
1979, Volume 15, Number 2, 136-138
DOI: 10.1007/BF00480352


Abstract
The photochemical chlorinatlon of tetrahydrofuran-2-carboxylic acid esters with chlorine at –15 to –20DaggerC leads primarily to the formation of 5-chlorotetrahydrofuran-2-carboxylic acid esters (70–80%). 4,5-Dihydrofuran-2-carboxylic acid and furan-2- carboxylic acid esters are formed as side products. The structures of the principal and side products were investigated by PMR and mass spectroscopy.



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DIRECT CHLORINATION OF SATURATED CYCLIC ETHERS USING TRICHLOROISOCYANURIC ACID
W. P. Duncan; G. D. Strate; B. G. Adcock
Organic Preparations and Procedures International
1971,  Volume 3, Issue 3, Pages 149 – 154
DOI: 10.1080/00304947109356057

Requested by POSEIDON




Synthesis of Quinolines and Their Characterization by 2-D NMR Spectroscopy
Abhijit Mitra and Ali Assarpour, Pamela J. Seaton and R. Thomas Williamson
J. Chem. Educ.
2002, 79 (1), p 106
DOI: 10.1021/ed079p106


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


ANTIMALARIAL STUDIES IN THE QUINOLINE SERIES
ALFRED BURGER, KENNETH C. BASS Jr., JAMES M. FREDERICKSEN
J. Org. Chem.
1944, 09 (4), pp 373–379
DOI: 10.1021/jo01186a009



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Design, Synthesis, and Structure–Activity Relationship Studies of 4-Quinolinyl- and 9-Acrydinylhydrazones as Potent Antimalarial Agents
Caterina Fattorusso, Giuseppe Campiani, Gagan Kukreja,
J. Med. Chem.
2008, 51 (5), pp 1333–1343
DOI: 10.1021/jm7012375

Magnetism in high-resolution NMR probe design. II: HR MAS
Doty,F;Entzminger,George;Yang,Y

Concepts in Magnetic Resonance
Vol.10(4) 1998 pp.239-260
DOI: 10.1002/(SICI)1099-0534(1998)10:4<239::AID-CMR2>3.0.CO;2-Y
http://onlinelibrary.wiley.com/doi/10.1002/%28SICI%291099-0534%281998%2910:4%3C239::AID-CMR2%3E3.0.CO;2-Y/abstract

Abstract

Various issues affecting nuclear magnetic resonance probe resolution are discussed, with emphasis on high-resolution or magic angle spinning (MAS) in this part. Symmetric positioning of chip capacitors at the magic angles addresses the largest B0 perturbation with ultra-low-inductance decoupling coils, and symmetric spinner drive designs with silicon-nitride coilforms are shown to be extremely beneficial in reducing spinning-, decoupling-, and variable temperature-induced thermal gradients. Other factors discussed include MAS sample cell design, high frequency (HF) coils, centrifugation, shimming, B1 homogeneity, B0 stability, and geometric compensation for variable angle spinning resolution.


Electronics and Radio Engineering: An NMR Probe Coil
Instrum. & Exp. Techniques
Vol.48(5) 2005pp.636-637
DOI: 10.1007/s10786-005-0112-0
http://www.springerlink.com/content/k50813163735k326/

Abstract

An NMR probe coil that produces a high-frequency magnetic field as uniform as the field provided by the well-known birdcage resonator, is described. Unlike the resonator, however, the coil can easily be tuned by varying a single variable capacitor.


Abstract

Monophenolic 2-amino-1-indanones and 2-amino-1-tetralones having various substituents on the nitrogen atom were prepared and their activities in vitro on D1 and D2 dopaminergic receptors were assayed. All compounds were inactive in binding assays and this inactivity is discussed.