Reactions of Vanillin and Its Derived Compounds. XXVII.1 Synthesis in the Syringyl Series
IRWIN A. PEARL
J. Org. Chem., 1957, 22 (10), pp 1229–1232


Abstract
Vanillin was converted to syringaldehyde by way of 5-iodovanillin in large-scale reactions. Electrolytic reduction of syringaldehyde yielded hydrosyringin which in turn yielded syringil upon oxidation with cupric hydroxide in acetic acid solution. Syringil was subjected to reduction under several reducing conditions to yield almost all of the possible monomolecular reduction products. Propiosyringone was reduced in alkaline solutions with sodium amalgam to yield a,a-diethylhydrosyringoin.

The Synthesis  of Syringaldehyde from Vanillin
J.M. Pepper & J.A. MacDonald
Can.J.Chem, 31, 476 (1953)[

ABSTRACT
Springaldehyde has been synthesized in high yields from vanillin. The process consists of the iodination of vanillin, followed by the interaction of the resultant 5-iodovanillin with sodium methoxide in anhydrous methanol at temperatures of 130 +/- 4'C. for one hour in the presence of a copper catalyst. Along with the Syringaldehyde, small mounts of unchanged 5-iodovanillin and vanillin were always found in the reaction mixture. Analysis of the final product was made by an initial separation of the components by downward paper chromatography using a mixture of petroleum ether (b.p. 100-120" C.), di-n-butyl ether, and water (10: 1: 1) as the developing agent for a period of 10 hr. The separated compounds were extracted from the paper and their concentrations in alcoholic alkaline solutions determined spectrophotometrically. Under conditions by which 5-iodovanillin was converted to syringaldehyde in better than a 95% yield, 5-bromovanillin gave only a 61% yield and 5-chlorovanillin gave no detectable amounts of syringaldehyde.

Separation of isopropanol from aqueous solution by salting-out extraction
Tang Zhigang, Zhou Rongqi, Duan Zhanting
Journal of Chemical Technology & BiotechnologyVolume 76, Issue 7 , Pages757 - 763,2001

Abstract
A novel salting-out extraction process has been developed to separate isopropanol from aqueous solution. Potassium carbonate was experimentally shown to be effective in modifying the liquid-liquid equilibrium (LLE) of an isopropanol/water/hexane system in favour of the solvent extraction of isopropanol from an aqueous solution with hexane, particularly at suitable salt concentrations. Potassium carbonate enlarged the area of the two-phase region. This effect essentially increased the distribution coefficient of isopropanol between hexane and water and increased the separation factor for isopropanol vs water, which is an important consideration in designing a solvent extraction process. The effects of potassium carbonate concentration, temperature and pH on the LLE were studied. Finally, a 30 mm × 1200 mm reciprocating plate column (RPC) was tested to separate isopropanol from an aqueous solution. When isopropanol in an aqueous solution with composition of isopropanol/water = 1:0.95 (wt/wt) was extracted by hexane assisted with 30% (wt%) potassium carbonate aqueous solution, the alcohol-water ratio increased to 11:1 in the extract.

Polyphosphoric Acids As A Reagent In Organic Chemistry
Frank D. Popp, William E. McEwen
Chem. Rev.1958, 58 (2), pp 321–401


I. Introduction.. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 321
11. Nature of the reagent . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 322
111. Cyclization reactions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 326
A. Preparation of heterocyclic compounds. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 326
1. Fischer indole synthesis.. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 326
2. Pomeranz-Fritsch reaction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 328
3. Synthesis of other nitrogen heterocycles . . . . . . . . . . . . . . . . . . . . . . . 329
4. Synthesis of sulfur and oxygen heterocy . . . . . . . . . . . . . . . . . . . . . . 342
5. Additional applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 345
B. Intramolecular acylation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3.4 9
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 363
2. Use of alcohols.. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 367
D. Miscellaneous examples of cyclization reactions . . . . . . . . . . . . . . . . . . . . . . . . . . . 368
IV. Rearrangements, . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 370
C. Cyclodehydration reactions of aldehydes, ketones, and alcohols. . . . . . . . . . . . . 363
1. Use of aldehydes and ketones.
A. Beckmann rearrangem . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 370
B. Lossen rearrangement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 374
C. Wagner-Meerwein rear . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 375
D. Schmidt rearrangement. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3 77
, , , , , . . , . , , , . , . . 377
VI. Other uses of polyphosphoric acid.. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 387
A. Nitration.. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 387
B. Bromination. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
C. Dehydration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
D. Hydrolysis. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
F. Phosphorylation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 392
G. Additional appli . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 392
VII. References.. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 393

Synthesis of deuterium labelled cocaine and pseudococaine
J. F. Casale, A. H. Lewin, H. T. Raney, D. A. Cooper
Journal of Labelled Compounds and RadiopharmaceuticalsVolume 29, Issue 3 , Pages327 - 335,1991

Abstract
Cocaine and pseudococaine were mass-labelled with deuterium at various positions on the tropane ring. The synthetic procedures followed were adaptations of those previously published for the unlabelled compounds. The isotopic purity was greater than 95% for 2-[2H]-, 4,4-[2H2]-, and 1,5,6,6,7,7-[2H6]-cocaine and 3- [2H]-, 4,4-[2H2]-, and 1,5,6,6,7,7-[2H6]-pseudococaine, while that of 3-[2H]-cocaine exceeded 90%.

   One pot synthesis of 4-methylaminorex
http://parazite.t35.com/hiveboard/novel/000458588.html

4-Methylaminorex Synth w/o CNBr
http://parazite.nn.fi/hiveboard/novel/000212038.html

Reduction of Salicylic Acid to Salicylaldehyde with Modulated Alternating Voltage
N. R. K. Vilambi and D. -T. Chin
J. Electrochem. Soc. Volume 134, Issue 12, pp. 3074-3077 (1987)


ABSTRACT
The effect of superimposing sinusoidal, triangular, and square-wave alternating voltage (aV) on the potentiostatic reductionof salicylic acid to salicylaldehyde has been studied. Polarization curves with aV modulation were measured withan amalgamated copper rotating disk electrode. Enhanced dc current densities were observed with increasing magnitudeof superimposed aV. However, aV frequency and type did not have significant effect on the resulting dc current densities.Batch cell electrolysis experiments were conducted with a H-type cell. The conversion of salicylic acid and yield ofsalicylaldehyde were measured as functions of electrolysis time, aV magnitude, type, and frequency. The superimposedaV significantly enhanced the reaction rate, conversion of salicylic acid, and the yield of salicylaldehyde. The energy consumptionof ac electrolysis was higher than that of dc electrolysis.

Electrochemical assistance of catalytic oxidation in liquid phase using molecular oxygen: oxidation of toluenes
Dorin Bejan, Jean Lozar, Gilles Falgayrac and André Savall
Catalysis Today Volume 48, Issues 1-4, 27 January 1999, Pages 363-369


Abstract
Liquid phase autoxidation of toluene and p-methoxytoluene in acetic acid has been studied under electrolysis in the presence of cobalt acetate. The latency period disappears when Co3+ is electrogenerated in the medium either before or during autoxidation experiments. The kinetics of the oxidation process is accelerated under electrolysis condition. The effects of temperature, current intensity, Co concentration, oxygen flow rate are investigated. The transition between the kinetic and the mass transfer limitations is determined in the case of p-methoxytoluene.

The methylenation of catechols
W. Bonthrone and J. W. Cornforth
J. Chem. Soc. C, 1969, 1202 - 1204,


Abstract
High yields in the methylenation of catechols by methylene chloride are obtained by using a polar aprotic solvent for reaction and maintaining low concentrations of the catechol dianion.

The Reaction of Vinyllithium with Tetraphenylphosphonium Bromide and the Formation of Phosphinemethylenes by RLi Addition to Vinylphosphonium Halides.pdf

Concerning the Mechanism of Formation of Triphenylphosphinealkylidenes.pdf

Studies in Phosphinemethylene Chemistry. XI. The Reaction of Alkyllithium Reagents with Tetraphenylphosphonium Bromide1.pdf

Studies in Phosphinemethylene Chemistry. II. Adducts of Triphenylphosphinemethylene with Boron Compounds.pdf

Studies in Phosphinemethylene Chemistry. XV. The Reaction of Tetraarylphosphonium Bromides with Vinylic Organolithium Reagents1.pdf

Studies in Phosphinemethylene Chemistry. IV. The Reaction of Triphenylphosphinemethylene and Triphenylphosphinevinylmethylene with Phenylbromophosphines.pdf

Studies in Phosphinemethylene Chemistry. III. Triphenylphosphinechloromethylene1.pdf

Studies in Phosphinemethylene Chemistry. X. The Reaction of Organolithium Reagents with Alkyltriphenylphosphonium Halides. The Mechanism of Phosphinemethylene Formation.pdf

A NEW PREPARATION OF TRIPHENYLPHOSPHINEMETHYLENES BY THE REACTION OF CARBENES WITH TRIPHENYLPHOSPHINE.pdf

 The stereochemical course of the conversion of 2-ureidoalcohols into oxazolidines. Part I.pdf

Studies in Phosphinemethylene Chemistry. I. Nucleophilic Displacement of Halide Ion in Metal Halides by Triphenylphosphinemethylene. A New Synthesis of Organometallic-substituted Phosphonium Salts.pdf

Studies in Phosphinemethylene Chemistry. XII. pdf


........can be found in the enclosed zip file