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Author: Subject: DMSO acquisition
3x
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[*] posted on 27-5-2006 at 16:10
DMSO acquisition


I posted this in beginings, but I will post it here as well. For those looking for DMSO, I have found out that MSM at health food stores is just DMSO2. Does anyone have a method to reduce it? This is pretty much the only way I'll be able to get DMSO, and I'm sure others are interested too.

EbC: title.

[Edited on 5-6-2006 by chemoleo]
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Sandmeyer
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[*] posted on 27-5-2006 at 16:38


There is no practical way to do this and even if it worked the idea of bying reagents from those sources is expensive. Anyways, if you need it for purpose of solvent look for alternatives, like dimethylacetamide or NMP.
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[*] posted on 30-5-2006 at 04:15


Are you in a city? I live in a suburb and if I drive maybe 5 miles, I have a source of DMSO 99.7%. If I drive into the closest city, there is another farm/agriculture store that sells DMSO 99.7%. It's not expensive at all. Look in the horse supply section.



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[*] posted on 30-5-2006 at 17:05


A local natural foods store in my area carries DMSO. The DMSO is sold for more $$ compared to the farm supply store that carries it. This is another option.
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[*] posted on 5-6-2006 at 06:16


Ya, thanks for the info, but this is for the international community. It's easy to get in the states, but not everywhere. I read somewhere on this site that their was a synth process for DMSO on the rhodium site, but obviously we are not getting it from there. Does anyone here have a simple synth?
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[*] posted on 5-6-2006 at 12:34


Why use a synth? Look on eBay. My search gave me around 20 suppliers of DMSO of varying purities and prices, who ship worldwide.

I purchased 3 bottles of 8 Oz of 99.9% DMSO. It freezes at 18C and that is not fun at all, but otherwise the stuff is quite good.

[Edited on 5-6-06 by woelen]




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[*] posted on 5-6-2006 at 15:40


First of all, thanks for moving this thread to the right place moderator/admin. I wasn't quite sure where to put it.

Second of all, unlike most newbies, I have searched for two weeks for a DMSO synth on google, here and the mirror sites of rhodium. I know I can order it, etc... Hence why I thought it might be useful to have a synth available for everyone on this site. It was mentioned in an old post on this site, but it refered to rhodium. After two weeks of searching, I figured it was time to ask.
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[*] posted on 5-6-2006 at 22:25


I found 99.9% DMSO at at a (Semi) local pharmacy for about $7 bucks. Unitednuclear has them for 18 bucks, which is a rip-off. Ebay has it for 9 bucks on average. Just look around.
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[*] posted on 5-6-2006 at 23:54


H. E. Roscoe, C. Schorlemmer - A Treatise on chemistry Vol 3 Part 1, London 1881, pages 213 - 214:
Quote:

Methyl Sulphide, (CH3)2S. In order to prepare this substance, Regnault recommends a solution of caustic potash in methyl alcohol to be divided into two nearly equal parts. The smaller of these is saturated with sulphuretted hydrogen and then mixed with the other part, so that potassium monosulphide is formed together with a little free potash but no potassium hydrosulphide. This solution is then saturated with gaseous methyl chloride, the solution gently warmed whilst the gas is being passed in, and the volatile product collected in a reservoir surrounded with ice. The distillate, which consists of a mixture of methyl sulphide and methyl alcohol, is next washed with water which dissolves the alcohol, the sulphide remaining insoluble. This latter is again repeatedly washed with water, and at last dried over calcium chloride.

Methyl sulphide is a colorless mobile liquid posessing an extremely unpleasant odour. It boils at 41C, and has a specific gravity of 0.845 at 21C. When allowed to drop into dry chlorine gas it takes fire and burns with a red flame with separation of carbon. Substitution products are however formed by more gradual action of chlorine, the last of which, perchloromethyl sulphide, (CCl3)2S, is a red liquid which decomposes on heating. Methyl sulphide combines with mercuric chloride, mercuric iodide, platinic chloride, and other haloid salts, and these compounds can be obtained beautifully crystallized from hot alcohol.


142 Dimethyl-Sulphine Compounds. Methyl sulphide combines directly with bromine to form the dibromide, (CH3)2SBr2, a compound wich crystallizes from water in amber-yellow octohedrons. If methyl sulphide be dropped into well-cooled fuming nitric acid, and the solution allowed to evaporate, colorless deliquescent needles of the nitrate (CH3)2S(OH)NO3, are obtained. If these are decomposed by barium carbonate, or if the bromide be decomposed by freshly precipitated oxide of silver, dimethyl-sulphine oxide, (CH3)2SO, is formed. This is soluble in water and alcohol and on evaporation and cooling solidifies to a colorless and inodorous mass. If the nitrate be heated to 100C, dimethyl-sulphone (CH3)2SO2, is formed. This is soluble in water and nitric acid, and crystallizes from the latter solution in prisms which melt at 109C although at 100C they begin to volatilize. This liquid boils at 238C.


That dimethyl sulphine-oxide is probably our DMSO. If you want to try this you need to do some research about toxicity, carcenogenity and other possible dangers of intermediate compounds.

[Edited on 6-6-2006 by chromium]
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[*] posted on 6-6-2006 at 00:52


US patent 2,581,050 is about making DMSO by catalytic oxidfation of dimethyl sulfide. Nitrogen oxide or nitrogen dioxide are used as catalysts. U.S. patent 2,825,744 deals with increasing of yields.

From 2,581,050:

Quote:

A current of oxygen at the rate of 370ml. per min. was bubbled through a 30cm. layer of dimethyl sulfide maintained at 26.5C, thereby producing a gaseous mixture containing the stochiometric amount of oxygen required for the oxidation of sulfide to sulfoxide. Nitric oxide at the rate of 30ml. per min. was added to the gaseous mixture as it passed into the first of a series of four reaction chambers, each consisting of a glass tube 4.3cm in diameter and 100cm in length. The reaction started immediately, the temperature of the reaction mixture reached a maximum of about 75C. In the first two tubes where most of reaction occured, and the reaction slowed down in last two tubes. The crude yellow product which dropped from the tubes, contained about 10 per cent dimethyl sulfide, about 2 per cent dissolved nitrogen dioxide, about 2 per cent of methane sulfonic acid, and some water. The crude product was refluxed at 100C for 30 minutes and the escaping gas was passed into the first reaction chamber. The dimethyl sulfide was removed by then heating the product to 150C, the methane sulfonic acid was neutralized by adding slacked lime, and the dimethyl sulfoxide was distilled in vacuum. The yield of pure dimethyl sulfoxide (B.P. 63C at 6mm. Hg) was 85 per cent of theoretical yield from the evaporated dimethyl sulfide.


[Edited on 6-6-2006 by chromium]
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[*] posted on 6-6-2006 at 05:35


Thanks a lot! Very helpful, and interesting... Some of those percursors are nasty!

Thanks again!

3x

[Edited on 6-6-2006 by 3x]
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[*] posted on 8-6-2006 at 23:34


Quote:
nitrate (CH3)2S(OH)NO3


Now THAT is interesting :)
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[*] posted on 17-6-2006 at 22:19


V. Richter - Organic chemistry, London, 1934:

Quote:

Sulphoxides and sulphones

These, as mentioned (p.172), result from the oxidation of the sulphides:

(C2H5)2S ---> (C2H5)2SO ---> (C2H5)2SO2

The sulphoxides are formed from the sulphides by oxidation by nitric acid or hydrogen peroxide (C(hemisches Centralblatt). 1909, I. 350). The unsymmetrical sulphoxides, R-SO-R', have been obtained in optically active forms, showing that three groups attached to the sulphur atom are not co-planar (J.C.S. 1926, 2079) (see p. 31). The sulphoxides are reduced to sulphides by nascent hydrogen.

Methyl and ethyl sulphoxides are thick oils, which combine with nitric acid to the compounds R2SO*HNO3. The free sulphoxides are regenerated from these salts by barium carbonate. Methyl sulphoxide is also obtained from the bromide Me2SBr2 and silver oxide.

The sulphones are obtained from the sulphoxides by oxidation with fuming nitric acid or permanganate, or from the alkali salts of the alkylsulphinic acids and alkyl iodides:

R*SO2K + R'I ---> R*SO2*R' + KI

They are not, however, the true esters of the sulphinic acids, but are very stable compunds in wich both alcohol radicals are linked to sulphur. They cannot be reduced to sulphides.
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[*] posted on 17-6-2006 at 22:48


F. C. Whitmore - Organic chemistry, 1947

Quote:

Alkyl sulfoxides, R2SO, are obtained by the action of nitric acid with the sulfides. The first product is a "nitrate," R2SO*HNO3 which is decomposed by water or mild bases. A better preparation is from the sulfides and an organic peroxide such as benzoyl hydroperoxide, PhCO3H. The lower sulfoxides are liquids which solidify on cooling. They are soluble in water, alcohol and ether. The higher ones are solids insoluble in water. Pr2SO m. 15C; Bu2SO m.32C; Hept2SO, m. 70C. reduction changes them back to sulfides.
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