05-05-04 14:44
No 505015
hay bees i was looking though rodiums site and found this does this have any truth behad it has anyone tryed or heard of this meothod because it seems pritty easy
STEP 1 (Makin' da nitroalkene)
Dissolve 1000 g of piperonal into 500 g of nitroethane containing 66 g of
cyclohexylamine and let the mix stand for about 3 weeks... Then, crush your
'chicken yellow' nitroalkene cake and wash it with about 2 liters of freezer
cold MeOH. Spread to dry...
YIELD: ABOUT 1000 TO 1100 g...
STEP 2 (Reducin' da above mentionned stufff)...
To 200 g of LiAlH4 dissolved in 10 L of ice cold anhydrous THF add dropwise
with cooling, 520 g of raw MDP-2-NP (straight from the previous step)
dissolved in 5 L of THF... The addition should take between 1 to 3 hours with
proper cooling of the reaction mix...
Stir at room temperature for 36 hours... (NO REFLUX!)
Then, add to the mix containing the now reduced compound, 1000 ml of IPA to
decompose the residual LiAlH4... followed by 400 ml of 15% aqueous NaOH...
Filter the solids (Al + Li salts) from the reaction mix and CAREFULLY wash
the filter cake using the remaining 5 L of THF from your 20 L drum...
Evaporate the solvents and crystalize the free base 'à la Shulgin' to get
about 600 g (between 500 to 700 g), of the product HCl.
YIELD: about 600 g of white fluffy stuff...
(Stranger)
05-06-04 04:33
No 505178
There is a synthesis in PiHKAL which looks pretty similar to this although i didn't check it 100% but yeah http://www.erowid.org/library/books_onli
(Hive Addict)
05-06-04 11:56
No 505259
That is quite an amount of white fluffy stuff you're about to synthesize. You must be one of these guys that adds MDMA instead of sugar to his coffee.
$UPPORT CRiME = $UPPORT THE GOVERNMENT
05-06-04 14:35
(Rated as: insignificant)
05-07-04 05:00
(Rated as: insignificant)
(acetaminophanatic)
05-07-04 08:36
No 505542
10 L of THF?
I wonder how big of a boom that would make upon the redistillation, if it had peroxides?
and that's a shit-load of LiAlH4, too.
Don't drop the flask....
Hmm...for a bee ready to drop that kind of gear, some careful checking at the hive could save a LOT of money, and maybe some lives....
THF --> other solvent = good
LiAlH4 --> other nitroalkene reduction method = very good
go search for sodium borohydride and catalytic transfer hydrogenation (CTH)...much cooler
and probably higher-yielding, too...
BTW, I might suggest saving that cyclohexyamine for other purposes. If you don't want it, I bet there are others who would pay much for it...
All in all, probably a workable but very "clandestine-unfriendly" synthesis. Too many watched, expensive, and dangerous chems. You can do better.
But what do I know of such things?
...it's an AOL chatroom for dyslexic spider monkies...
(Stranger)
06-07-04 05:54
No 511884
I realize Anhydrous THF and LAH are very expensive. Has anyone tried any substitutions with success? LAH is going for $1 USD/gram. Cyclohexylamine is dirt cheap but Anhydrous THF is pretty expensive 25 liter 229.00 USD. Buying nitroethane is a bitch most people think you are a terrioust just mentioning it. But it is not imposssible to get. Just curious why not use nitromethane? It is much easier to get.
(Chief Bee)
06-07-04 16:22
No 511976
Just curious why not use nitromethane? It is much easier to get.
Because the resulting nitroalkene would give the inactive MDPEA after reduction, and not MDA.
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