07-15-03 09:28
No 447503
Confident in achieving ketone via the perfomic route, if that was as far as one needed to go then I’d be stellar.
Tried a MM al/hg reduction in a 1 liter trial size, cut amounts of chemicals in half as well. Kept addition rate at 40 minutes; after reaction smelled like methylamine and I thought that something had to be in that sludge.
Washed toluene was not perfectly clear and looked like something was ready to fall out of it.
Gassed without drying HCl and used Epsom salts dried at 190C
Toluene thus turned reddish and red oil appeared at bottom. Foiled again I thought, dam water must be the culprit, also my impatience after dreaming for 52 consecutive hours.
The chemistry window had closed and I bottled the 300mls of reddish toluene with red oils appearing at the bottom in a flask.
Then used TFSE to find posts regarding this: No 387066 No 391978 No 342884 No 186734 etc.
Comment: I will most def. do an A/B extraction and anal retentive drying of this system to recover anything present.
Question: I have to wait a month for the chemistry windows to reappear and was wondering what is the stability of mdma in this retched environment? I will at least get sleep knowing it can be rescued later and is not all decomposing or something. Also the posts of what this red oil absolutely contains are uncertain. I know the pros deal with actual crystals and not this shite, but what really is this, water/fb/HCl ?
Thanks for comments, conjectures, and time
Oh in random thought, using dry ice to concentrate H2O2 following phase diagrams works great.
(Hive Bee)
07-15-03 12:00
No 447536
Could the red shit be unreacted mdp2p? How long was your reaction?
(Stranger)
07-15-03 12:29
No 447542
It very well could be, but I would hope that some ketone was reduced to amine though. I coming from the angle hey "some" reaction happened, equilibrium shifted in favor of amine, maybye not best yield though.
I wish I could run HPLC on the stuff and really find out!
Simply for the sake of me and every other newbee that runs into it.
But what conditions will break down the little mdma that potentialy formed in the reduction? Will over gased toulene with some water be harmful to our precious? I dont wants to harm the precious. But the mines of Mordor are a months journey. Im sure Gandelf could calm me down with some herb.
(Hive Bee)
07-15-03 12:59
No 447546
Well if it is mdp2p i shouldn't have to say it should be refrigerated until further dreaming which sucks seeing that the dea also knows it needs to be refrigerated always take precuations and know that even your fuck up's can land you in prison with good ol' nasty nate if any trace amounts can be found
(Hive Addict)
07-15-03 13:42
No 447555
If the MDP2P didn't react to form the imine, then when it went through the Al/Hg it would have formed MDP2Pol. Let's hope that didn't happen. But what it sounds like to me is that you got MDMA freebase, but when you tried to gas, you didn't dry everything properly, and so the MDMA*HCl formed a red tar with the water. Just do an acid/base, then gas again, this time with proper drying, you should get most if not all of your product back. Or you could just extract the toluene with some HCl solution, and the evap down to the red tar, then add some acetone, and you would get your crystals. But if you try it that way, you won't really get as pure of a product. It's up to you. But I'm reasonably confident that the product you have now will store fine until you have a chance to try and rescue it.
It is seductive, way too seductive. -Eleusis
(Chief Bee)
07-15-03 22:54
No 447710
After an Al/Hg reductive amination A/B extraction is a must, and should very very preferable be vacuum distilled before you gas it. If you skip the distillation, it is mandatory that you recrystallize the MDMA.HCl afterwards.
(Hive Addict)
07-16-03 12:40
No 447832
and chill your toluene/oil mix to 0C or so,before gassing,otherwise crystals don't come out and it may form a red bottom layer like that.
For those about to synth,we salute you