04-17-03 06:38
No 427484
I have had a few problems with making mdma and wondered if
I could get some advice from some fellow bee's
I have gone for a performic route and then a al/hg reduction
Isomerisation of safrole with NaOH and CaO iso (i think)
came over between 238 and 250C I lost a lot trying to
seperate the CaO from the solution.
next I mad formic acid by Oxalic and glycerole heated to
110C then purified to 70 to 77% via azeotrope boiling point.
(I can get boric acid if boric anhydrided is a better aproche)
I have 50% peroxide so I did the math to make it the same
as a 80% 30% mix.
I distilled DCM from paint thinner then did the epoxidation
via shaking the hell out of it in a flask with a reflux condensor. It heated up nicely to a reflux
and the oil layer went a
nice orange and the water layer went a pail yellow.
next I did a 3 and a half hour reflux in H2SO4
shaking the flask so as the two layers mixed the whole time.
on distallation my vacume pulled somthing over at 190C
(safrole comes over at 142C) I think this is too high for
ketone but I kept pressing on thinking that it was either
fucked or it wasont (methylamine is cheap to make so it
didont worry me to much)
I made the methylamine with hcl and hexamine cleaning it
with acetone to remove hexamine then doing a recrystaliztion
in ipa. the flakes that came out looked like fish scales
and glittered in the light.
I made my HgCl by braking a thermometor into boiling sulfuric acid
then poring off most of the acid after a few minutes.
I then used bicarb to nutrolise it then added hcl.
al was made out of crushed squares taken from pie trays.
the alcohol for the amalgum was ipa.
I shook it through out the entire 6 hours.
so finaly I get to the end and do an acid base in my sep funnel.
there must have been some hexamine still in there as a heap
of white fluff fell out of the solution.
after two a/b's I had an oil and a methylamine smelling liquid.
doesnt only nitrogen compounds come through a a/b
the oil was not mdma or only had a small amount in it.
the oil must have been a nitrogen compound but what I dont
know.
I have brought the stuff to set up overhead stirring so
as to mix things better and I have found a source of KOH
any other problems here that anyone can see.
thanx for any help I get.
e3500 console login: root
bash-2.05#
(Hive Addict)
04-17-03 07:21
No 427490
A for effort !
what makes you think that what you have isn't x? describe in more detail how you worked-up the Al/Hg rxn. and describe at what point you had "white fluff 'falling out of solution.
also if you have any of the ketone left, get some sodium metabisulfite at a wine brewing shop and run a quik bisulfite test, then you will know more precisely where things may have gone wrong
(Hive Bee)
04-22-03 09:36
No 428584
i nuralized the oil and then did the dodge tast test.
figured it would either be active or none active
got a bit of a somach ache from it and little high
but not much.
as far as when the fluff fell out it was
in the acid part of the ab.
when I pulled the oil out with base no fluff
when I pulled the amines out with acid from the non polar
bang white fluff just like when I synthed methylamine.
just got some metabisulfite
e3500 console login: root
bash-2.05#
(Hive Bee)
04-28-03 08:42
No 429923
good thing you didn't breathe some SO2 and die...
i'm surprised you got any HgCl2 at all from the haphazard procedure you described.
but, it works you say? the aluminum turns grey and breaks down?
swim has found HgI2 much safer to make at home...
sounds like you ketone BP is okay, try gassing the mdma freebase out of anhydrous toluene or xylene.