Author Topic: A/B HELP!!! After i added 100ml of 10% HCl to ...  (Read 773 times)

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methlab

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A/B HELP!!! After i added 100ml of 10% HCl to ...
« on: February 12, 2004, 11:02:00 PM »
Hi! I added 100ml of 10% HCl to the Toluene/Freebase mix, to start my A/B. I swirled it for 20 minutes then i wanted to separate, but could not, because there are 10cm of white christals on the bottom of my beaker !!! What has happened? I have never seen this before. Did the MDMA chrystals crash out of the solution? Normally i then add the NaOH, washe with clean NP, then extract , dry and gas...  :(

Purepacker

  • Guest
No idea
« Reply #1 on: February 13, 2004, 12:12:00 AM »
But when you acidify MDMA freebase you basically are preciptating MDMA HCl crystals. Since you add a lot of water I believe a large part of these will dissolve. I find it hard to believe the water layer is saturated with MDMA HCl, so that´s not an explanation. What was the volume/concentration of the TOL/BASE mixture? And did you check pH of TOL/BASE mixture before and after addition of HCl?


methlab

  • Guest
did it as allways
« Reply #2 on: February 13, 2004, 01:14:00 AM »
Hi! I did not check the PH, i did it as allways. It has never failed. Today i used Nitroethane instead of Nitromethane, but this should not be the problem. I did just a small batch, there was 10g MDP2P left and i thought i should try making MDEA. I added 60ml from the 100ml 10%HCl to about 250ml Toluene/Freebase mix to get the salt into it. The solution started to get milky white, filtered and got a whole coffeefilter of white stuff out of it. Don't know what this is, think this is not edible. Will save everything until tomorrow, maybe someone had a similar experience. Otherwise it's for the toilette... :(

hsark

  • Guest
just a guess...
« Reply #3 on: February 13, 2004, 07:24:00 AM »
swim thinks that if you have solids just remove them and continue your a/b. if after you distill your solvent you have an oil your good to go, but its best to distill oil too. if your paranoid you could always wash more than once. if this is your first time with this reaction maybe the solids are normal. but if not something probably affected the reaction. good luck.


gsus

  • Guest
whatthefuck
« Reply #4 on: February 13, 2004, 09:56:00 AM »
are these solids sol in fresh 5% HCl? in H20? in hot alcohol your choice? if not you should see big red flags.

methlab

  • Guest
filtered them out
« Reply #5 on: February 13, 2004, 02:37:00 PM »
I have done a lot of A/B's for purification, but this has never happened before.
I filtered the white crystalls out and let them dry, got 1/2 coffeefilter full of white crystals (from 10g MDP2P), but they are mixed with toluene now. How can i purify these crystals, wanted to convert them back into freebase, but they are not soluble in water/acid/NaOH, i think this is because of the toluene.
I continued the A/B after filtration, but i got just 2.5g out of it (MDEA). Is the rest for the toilette? Is MDEA so different from MDMA? :)

gsus

  • Guest
solvent of cyrstallization
« Reply #6 on: February 13, 2004, 11:36:00 PM »
if you've heated the crystals, for long enough, they dont contain solvent any more. i would not heat these crystals in anything sensitive to explosions, and would be wary of grinding the dry crystals, just in case. use the H2SO4/HCHO reagent to color test. look up marquis / MDMA in TFSE if you haven't done this b4. course these might contain enough to give pos test tho not real pure. if it explodes on contact w/ the reagent it wasnt X. I know you know what youre doing but shit happens. even prize-winning chemists like not me get craptacular results sometimes. hopefully no one is putting things in toluene.

hsark

  • Guest
agree with gsus..
« Reply #7 on: February 13, 2004, 11:44:00 PM »
but if its not soluable in whater its not mdea hcl. its more than likely trash or a byprouduct that you dont want to eat.


methlab

  • Guest
it was for the toilette
« Reply #8 on: February 15, 2004, 01:52:00 AM »
i checked the dry 'crystalls' but this was not MDEA, it was trash, discarded it. maybe there went something wrong during al/hg. this time the alufoil nuggets did not start to float, even after 40 minutes amalgamation. maybe i have nuggetized them too much. what will happen in such a case? if the foil is nuggetized too much, can this prevent a removing of the oxidized alu ?