Dope Amine
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Removing Sulfur Compounds from Dehydrogenation Reaction Mixture
I used sulfur in a dehydrogenation/aromatization reaction and I'm now trying to figure out the best way to remove the sulfur byproduct impurities.
The first thing I did was dissolve the reaction mixture in methanol and then gravity filter through DE. This removed the yellow sulfur color but the
sulfide smell remained. Activated carbon was tried but it didn't seem to do anything useful. When the methanol was rotovaped the majority of the
sulfides seemed to carry over with the methanol but the product still smelled bad as well. Hydrogen sulfide has a very potent smell, in case you
weren't aware.
I came across a literature reference where after the dehydrogentation reaction they dissolve the mixture in benzene and then filter through a small
column silicic acid. I had never heard of this chemical before and I have no idea how it might work but I went ahead and ordered it to give it a try.
Can anybody suggest an efficient way of removing the sulfur byproducts in my reaction mixture? Do you know how/why silicic acid would help with
purification?
Thanks!
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fusso
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What about extracting the H2S using acidified Cu2+(aq)? The Cu2+ will react with H2S to ppt out CuS and you can filter that out. What compound were
you trying to make?
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Dope Amine
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Thanks for your suggestion! I am converting THC for a CBN for a legal cannabis company. Maybe I can flood a methanol solution with the aqueous
copper reagent and see if that properly removes the hydrogen sulfide smell.
If anybody has any knowledge regarding the efficacy of silicic acid or how it works it would be appreciated.
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