06-10-03 04:11
No 438959
I have finaly got around to salting my ketone with bisulfite
and there is no problem there.
when using nitromethane in the amalgum I get a methylamine
smell and no mdma
is this the way I am extracting it from the sludge
I have been using a buchner funnel with minimul NaOH
I get a light yellow liquid and when I a/b then gass
I get few if no crystals.
boiling down the contents of the amalgum some times gives
me ketone and sometimes nothing.
I have found that if I use extra water in the amalgum I
get nothing and if I use anhydrous conditions I get my
ketone.
could it be that I am throwing my e down the drain with
my sludge becouse I havent used enough base.
will base hurt mdma if it is in excess.
if I can not get this to work I am going to move to either
a lukart or a NaBH reduction.
also can you use ammonium acetate or formamide in the
Al/Hg to make mda.
any help would be much apreciated as this is costing me heaps of time and precursors.
thanx
Q
e3500 console login: root
bash-2.05#
(Hive Addict)
06-10-03 05:15
No 438966
Is your reaction exothermic? I have found out that if the nitromethane reduction isnt exothermic, the reaction actually failed.
You need to basify just enough to make the pH about 10. Too much pH and you destroy the molecule.
Next time you do an A/B procedure, slowly....i mean slowly basify one drop at a time with good stirring. this will first make a cloud then when the oil falls out, let it settle for a few hours. Then extract with DCM 3x, combine extracts, distill off DCM, and weigh out the crude base. Then you should distill if your yields are high enough. If you collected very little after a failed reduction, then check your MDP2P, most likely you didnt create real MDP2P.
Good luck~
(Hive Addict)
06-10-03 09:35
No 439000
Too much pH and you destroy the molecule.
Bull...i've never seen anybody destroy MDMA molecule with NaOH or KOH solutions.
this will first make a cloud then when the oil falls out, let it settle for a few hours.
Yes it goes cloudy but in raf's experiences oil floats rather than forms a bottom layer
Then extract with DCM 3x
These extractions might not be needed as freebase is not soluble basic water and forms it's own layer in no time.If you still think they are,wash once,three times is definitely overkill.
For those about to synth,we salute you
(Chief Bee)
06-10-03 14:33
No 439041
These extractions might not be needed as freebase is not soluble basic water and forms it's own layer in no time.If you still think they are,wash once,three times is definitely overkill.
That is very bad lab technique, and you will lose product by not extracting with DCM. Also, if you have alcohol still in the solution, the freebase will have a significan solubility in the aqueous layer.
(Hive Bee)
06-10-03 16:21
No 439065
raffike: You stated the oil floats for you? Is this from the standard MM Al/Hg reduction?
SWIM has only 2 experiences in the area, but his sinks and forms a nice layer below.... Shouldn't this be quite a standard thing?
SWIM uses dilute 5%HCl to acidify, 35% NaOH to basify.
(Hive Addict)
06-10-03 16:45
No 439069
Raf uses methylamine but that doesn't really matter.Maybe it depends on how much of base do you as stronger base solutions are denser than weak solutions.Does anybody know MDMA fb density?It's somewhere between 1.1 and 1.2 methinks.Strong NaOH solutions may be denser so freebase floats on theem.
For those about to synth,we salute you
(Hive Bee)
06-11-03 03:14
No 439236
My last few times running I've noticed the floating/falling of the oil depending on the base concentration, how much MeOH is in the solution too. Have had it float and sink. This may not help you, but ketone that has not been distilled has consistently yielded a freebase with lower density than the ketone. Ketone averaging between 1.18 to 1.189 and freebase post al/hg ~1.15.
Raffike. I've always wondered, given al is completely broken down, is there really a need to use NaOH when using MeAm because the post reaction mixture was always ~10.5 to 11 anyway.