but further down in the same thread (barium's):
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Sunlight
(Pioneer Researcher)
07-08-03 18:40
No 445732
Test with 3,4,5 TMB failure Bookmark Reply
Acording with Barium's instructions, 5 gr of 3,4,5 TMB was mixed with repective amounts of aqueous methylamine and nitromethane in 20 ml of methanol, and it was kept at 50 C for 1 hour. Then it was put in the freezer, and filtered. The filtrate was a yellow and amorphous solid, and a TLC showed three spots, one on the bottom line, other in the place of the aldehyde an the third one in the place ot the nitrostyrene.
I tried to recrystallize a sample of 1.9 grams in ethanol. It was posted a reference it the Hive in wich this recrystallization was done using 7:1 of ethanol, but this substance refused to dissolve even in 18:1 boiling ethanol. I filtered it immediatly and recovered about 1.2 grams of the product, a sample of that couldn't be dissolved even in a large excess of boiling acetone, while a sample of the nitrostyrene made with Shulgin's procedure (one spot TLC) was easily dissolved in a bit of acetone at room temperature. The procedure yield a mixture in wich the main part corresponds to this not soluble product, that appears in the bottom line in the TLC because it is in suspension. I got the same product when I tried to make 3,4,5 TMNS with cyclohexylamine in methanol at room temp as I've said before, then I was confused thinking it was the styrene, because it has a yellowish aspect.
So I don't recommend this method if you want to get this particular nitrostyrene. It probably will work fine with some aldehydes, but others will produce byproducts, as in this case and in the others tested in the paper in Rhodium's page. (Link above).
I guess Barium didn't verified that the product he got in his test was the desired product.
By the way, I guess there is a typo in PIHKAL in the entry of mescaline, the nitrostyrene is recrystallized using 15 ml/g but in fact 5 ml it's enough, I've done it. There's another one in the dose, the amount of the sulfate and the hydrochloride doesn't match.
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still looking for the most promising 3,4,5 cat.!