12-27-03 12:00
No 479344
SWIM just had his first dream and wanted to thank everyone here! After researching and UingTFSE many times was able to get everything right. SWIM froze sassy then did a distillation on it to clean it, did the Benzo Wacker which also went really smoothly, was able to get 110g of MDP-2-P; followed that up with MDP-2-P w Al/Hg + MeNO2 which went well till gassing and SWIM oiled it out, thinking that SWIM messed up, that batch was dumped and after some more searching found out how to fix that problem but it was too late. SWIM tried again this morning and had a wonderful success! SWIM though that some how water was getting into the tolly during the gassing so SWIM setup a 2 stage filter, dripped H2SO4 onto NaCl w HCL that bubbled through H2SO4 that went through a colum full of CaCl into the tolly, after gassing 3 times filtering and washing with acetone and drying SWIM had a total of 18.3g
THANK YOU ALL!
Hope everyone had a happy holiday!
(Newbee)
12-28-03 18:05
No 479554
thats cool. btw did you distill the 110g of mdp2p before using it.
(Stranger)
12-29-03 12:25
No 479665
must have been with vac - temp about 130-150C at 15 mm Hg - me thinks
(Stranger)
01-01-04 14:58
No 480142
SWIM didn't re-distill his MDP-2-P, the for run was dumped and the rest all came over between 174-177 at 26.5" of Hg. <Not sure how accurate the vacuum gauge is, currently using and aspirator, SWIM just received his new vacuum pump and is looking forward to using this to raise his vacuum to closer to 30” of Hg>.
SWIM has been doing some more reading and is really interested in higher purity of product, SWIM has read many posts on recrystallization and want to make sure SWIM gets it right. This is what SWIM plans to do.
1. Add 500 ml isopropanol to a 600 ml beaker and bring to boil
2. Add MDMA.HCL to 250 ml beaker, pour hot isopropanol into beaker to dissolve MDMA.HCL
3. Let cool to room temp
4. Filter
5. Wash crystals with some acetone
6. Do a second recovery by placing first wash in freezer and repeating <Second crystals may/will be less pure>
Has SWIM missed anything there?
Also SWIM would like to distill off the toluene/xylene before gassing and wanted to make sure SWIM doesn’t mess this up either.
So once SWIM has everything ready to gas, toluene (or xylene) can SWIM just throw the mixture into a distilling flask and distill off the toluene/xylene? SWIM sees that toluene should come over at 110 degrees, and xylene at 144/139/138 depending, how much toluene/xylene + MDMA.HCL freebase should be left in the flask for gassing? ~100ml?
Is this a safe method? SWIM plans on doing this under vacuum and will calculate what temp the toluene/xylene will come over at <guessing for ~27” Hg ~45 degrees for tolly and ~75 degrees for xylene>
SWIM was also thinking about doing an A/B extraction and moving the freebase into the DCM and the distilling of the DCM and gassing the DCM, but read a few posts that said gassing the freebase in DCM had poorer yields than gassing in the toluene.
If SWIM plans on doing 2 recrystallization would you still recommend doing an A/B extraction before gassing?
All suggestions welcome.
Thanks.
(Stranger)
01-01-04 18:27
No 480166
First off, congrats. I remember what it was like for me and that was a while ago before the benefit of sites like this. I had to learn on my own. I still say a prayer for all the sacrificed sassy trees that were donated to the cause.
First of all, I always use acetone for my crytalization with HCl gassing. I've never had to re-crytalize but i have to admit often I don't get full crystalization and have to evaporate the acetone to get the crystals out. But acetone is cheap, I don't like toluene and i prefer to get as many of my supplies as possible from regular stores rather than chem suppliers.
But as you get experience you will learn much. The method that you produce you MDP2P can affect all sorts of thing down the line.
Happy new Year.