3x
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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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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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DDTea
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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.
"In the end the proud scientist or philosopher who cannot be bothered to make his thought accessible has no choice but to retire to the heights in
which dwell the Great Misunderstood and the Great Ignored, there to rail in Olympic superiority at the folly of mankind." - Reginald Kapp.
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DeAdFX
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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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3x
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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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woelen
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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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3x
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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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alyks
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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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chromium
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H. E. Roscoe, C. Schorlemmer - A Treatise on chemistry Vol 3 Part 1, London 1881, pages 213 - 214:
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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.
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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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chromium
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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:
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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.
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[Edited on 6-6-2006 by chromium]
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3x
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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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=SkyNET=
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| Quote: | | nitrate (CH3)2S(OH)NO3 |
Now THAT is interesting 
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chromium
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V. Richter - Organic chemistry, London, 1934:
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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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chromium
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F. C. Whitmore - Organic chemistry, 1947
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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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