The Vespiary

The Hive => Methods Discourse => Topic started by: mtnfrogger198 on March 20, 2003, 11:56:00 PM

Title: Hot or Cold?
Post by: mtnfrogger198 on March 20, 2003, 11:56:00 PM

For anyone who has succesfully synthesized MDMA via the Al/Hg/Nitro method...

Is it better to do it with or without external cooling?

Title: With cooling defintely.
Post by: hCiLdOdUeDn on March 21, 2003, 01:04:00 AM

With cooling defintely. Never do a reaction without cooling because the reaction can literally explode. Boiling methanol/ketone mixture is not healthy to breath. Its good for the reaction to be hot but not out of control. Just keep practicing you will get there. . . ;)

Title: Just Chillin...
Post by: mtnfrogger198 on March 21, 2003, 01:12:00 AM

Yeah, that's what I thought. I did it with my precious reflux condenser tube, so not a single vapor escaped.

I was just worried that I let it get too hot, burning up my product. Next time, I'm gonna try a water bath, but not ice water.

Title: You cant really "burn" up your ...
Post by: hCiLdOdUeDn on March 21, 2003, 05:42:00 AM

You cant really "burn" up your product because the methanol would have to boil away first.

I am positive you can get back your mdp2p after extraction and re-distilling.

Title: No, any MDP2P which didn't form MDMA must have
Post by: Rhodium on March 21, 2003, 11:00:00 PM

No, any MDP2P which didn't form MDMA must have been reduced to MDP2Pol.

Title: Fuck
Post by: hCiLdOdUeDn on March 21, 2003, 11:03:00 PM

This explains why swim gets lower yields on the second amination after trying to extract MDP2P from a "failed" amination. Fuck Fuck Fuck. Only if I had known this earlier. Thanks rhodium again.

Title: reduction of glycol by Al/Hg
Post by: goiterjoe on March 22, 2003, 08:35:00 AM

if the glycol was to be mistakenly used in a reductive amination run, would it most likely be first converted to the epoxide and then reduced to the alcohol as well?  Would it most likely form as MDP1Pol instead of as MDP2Pol?

On a tangent thought, if this alcohol were to be attacked by anhydrous HCl gas such as if it were dissolved in Toluene during gassing, would it be very likely that it might react with the HCl to form that red "oiling out" product that has been commonly described here by people who didn't reflux their epoxide/glycol in sulfuric acid long enough?  I think the sulfuric acid reflux reaction is one of the most commonly messed up reactions among many chemists here.  The only writeup I have gotten to work consistently is the one in Shulgin #109, and many people here have claimed he used twice as much as he needed.  Sometimes other people's advice can be dishearteningly expensive.

Title: If the glycol was subjected to an Al/Hg ...
Post by: Rhodium on March 22, 2003, 08:36:00 PM

If the glycol was subjected to an Al/Hg reaction, it would likely remain unchanged afterwards and be removed in the A/B.

Title: glycol to epoxide formation
Post by: goiterjoe on March 22, 2003, 09:22:00 PM

would the glycol be converted to the epoxide when exposed to heavy basic conditions during the A/B process?

Title: Probably not to any greater extent during such
Post by: Rhodium on March 23, 2003, 08:08:00 PM

Probably not to any greater extent during such a short duration around room temp.