Author Topic: Al/Hg Nitro of mdp2p... a step up???  (Read 2715 times)

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AngelX

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Al/Hg Nitro of mdp2p... a step up???
« on: October 29, 2003, 04:58:00 PM »
whats up beez
i've done much reading on this forum, and many other places. I have had many a good dream about the al/hg reductive amination many times now, yielding on average 20 grams of mdma.hcl from 25g ketone. Now i am taking things a step up. I am running a reaction in a 5 gallon water container, with a pvc drain valve so i can even extract the toluene in the container. Then i just drain off. This reaction is 10x that of methyl man's writeup, and I was wondering of the molar ratios to be used in such a large scale reaction, as i dont want it to run too fast. Should i use thicker aluminum... and what about the amount of Mercuric Chloride??? any info will help, as the largest amalgamation if have successfully dreamed to date was for 125g mdp2p.

Midi

  • Guest
Hes Big!
« Reply #1 on: October 29, 2003, 06:02:00 PM »
I hope you have a serious stirring mechansim and a shit load of industrial fans.  ;)

Should i use thicker aluminum... and what about the amount of Mercuric Chloride???

The amount of mecuric chloride is relevant to the amount of time you want to wait for the al to amalgamate. You could use 1g per whatever and amalgamate everything in 20 minutes, or use .5g and have it ready to go in an hour. If you have time use less.

with a pvc drain valve so i can even extract the toluene in the container

Chances are that toluene is going to eat your vessel, or something similiar. Whats wrong with a 12L rbf 45/50 center joint?


AngelX

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In reply, no the toluene will not eat the...
« Reply #2 on: October 29, 2003, 07:24:00 PM »
In reply, no the toluene will not eat the vessel. It is a synthetic resin base, and all joints are connected with either abs or poly-vinyl with heat resistent epoxy, which is also no soluble by non-polars. There is nothing wrong with a large flask as you have said, but i have a drain valve mounted at the exact point after i basify, so when it comes time to extract, all i do is open the valve, and the NP comes out in a gentle stream, no fuss, no mess, no sep funnel.

When i get the chance i will post a pic of the vessel, along with a 3 gallon bucket i have set up for my slight variation of MM's safrole wacker via quinone in methanol. It works quite well for the same reasons as this reaction.

Maybe i should rephrase my first question. How thick should the Al be, and how much HgCl2 in ratio to not let reaction run away. I have read that at this large scale the reaction could get out of control, and that is quite a bit of nitromethane to have fizzing all over my perfect dream!!!
Thank god i dont smoke! ;)

Vitus_Verdegast

  • Guest
UTFSE
« Reply #3 on: October 30, 2003, 05:55:00 AM »
This might be helpful to you:

Post 382493

(abacus: "Processing  1 Mole Ketone Using Nitromethane", Methods Discourse)


about thickness of foil:

Post 466652 (missing)

(hypo: "which al/hg !?!?", Newbee Forum)



Antibody2

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baal chemist ran a huge rxn in a 55gal drum...
« Reply #4 on: October 30, 2003, 09:40:00 AM »
baal chemist ran a huge rxn in a 55gal drum with presuure release valves and the whole deal, should read his write up


baalchemist

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After that initial 1/2kg run in the 55 gal.
« Reply #5 on: November 10, 2003, 02:09:00 AM »
After that initial 1/2kg run in the 55 gal. drum, Baal started making preparations for a 1Kg run. Unfortunately Baals mother's cancer suddenly took a turn for the worse & I went to care for her in her last couple of months over in a neighboring state, so it was put on hold. When I returned, I was too depressed & not functioning that well  mentally so I decided to scrap the whole 1Kg idea for safety concerns. I still have the drum in storage, just maybe..... I had even installed 1"copper tubing wrapped around the upper half of the drum and that fastened to a steel chamber that I mig-welded to the lid. This all served as the condensing apparatus. The damn thing weighs a ton now and reminds Baal of the robot from 'Lost in Space' for some stupid reason.