Hi, swim is new to this forum. Swim has played around with Bandil's
recipe at the-hive quite a lot a few months ago. Got good results.
But now that the site is down swim can't remember the full
procedure. Does anybody have it (it's the one
Bandil calls shake and Bake). Please please help a bee find its way
back home..
One pot synthesis of 4-methylaminorex
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Hi!
Further exploration of an initial suggestion by Rhodium - to
perform both the preparation of the carbamoyl norephedrine as well
as its cyclization to trans-4-MAR in one pot gave the following
results:
Theory:
When the initial norephedrine hydrochloride is mixed with potassion
cyanate, it forms the carbamoyl coumpound in near quantitatie
yeilds with respect to the norephedrine. The original patent's uses
a slight molar excess of the cyanate in order to give complete
conversion. When the first reaction is done, there should thus be a
mixture of: N-carbamoyl-norephedrine, potassiumchloride and traces
of of cyanate. The remaining cyanate will be destroyed by the huge
excess of acid which will be added later. In the end these
impurities should have no influence of the ring formation,
catalysed by the acid. It should in theory be possible to do the
initial reaction and simply add the acid in one portion while
heating continusouly till the reaction is over. With this in mind,
it seems kind of a waste to isolate the intermediate, so this has
to be tested :)
Practice:(in theory of course)
5 grammes of norephedrine.HCl(26,5 mmoles), was placed in a 100 mL
FBF, and 2,3 grammes of KOCN(28,4 mmoles) and 25 mL's of distilled
water was immediately added in succession. This was heated to
reflux directly on the hotplate for two hours.
After this time, 30 mL's of 2M HCl(60 mmoles) was added. This
caused a bit of bubbling(probably from the excess cyanate being
broken down to gasseus -i-cant-remember-what-). Reflux was
continued for an additional two hours. The mixture took on an ever
so slight pinkish tint, which the "old" synth also tend
to do at this stage.
After 2½ hours of reflux, the mixture was cooled and basified with
sodium carbonate and presto a lot of pretty white crystals
precipitated on the bottom of the beaker. The yeild looked like
that which is expected from the normal reaction. They will be
measured shortly.
Conclusion
Total success!!
We'll the usual cyanate route to 4-methylaminorex was easy, but
this is more like baking a shake-n-bake cake really ;)(which is VERY
easy if you didn't know). Bioassay's are pending though, but
nothing that was put into the flask would have reacted the way, the
final product did. The yeild will also be measured shortly!
T_C - never been lucky enough to find any but
it has come up a few times in forums recently and an unfortunate
member of another board was busted recently while in the process of
dreaming some up... Poor guy.
Anyways - http://www.erowid.org/
is an amazing source of info on various plants, chems and so on...
"Life
should not be a journey to the grave with the intention of arriving
safely in an attractive and well preserved body, but rather to skid
in sideways, cigar in one hand, favourite beverage in the other,
body thoroughly used up, totally worn out, and screaming WOW - What
a ride!"
Yeah, that is where switc googled too, switc
thinks she may have had some of this, the tannish tint is what
makes switc think this. How is it made in laymens terms? Anyone?
From pseudo, it says norephedrine but how the hell do you get there?
And the other chems., are there OTC supplements?
1/10 of a gram (100mg) is to much if its the
pure base. 1/50 of a gram (20mg) is advised and usually enough even
for 90kg males.
The dosage is actually a problem, best
way is to weigh out a gram and to dissolve this in booze and to
part the booze into 100 portions and to drink one or two a time.
Yes! There is one liter booze required and one portion is 10ml.
The effect is the same and you wont feel
short-tempered except you are a short tempered person anyways. For
help with "short temper" (and many other personality
disorders) I advise to join a tibetian monastry for seven years -
this helps guaranteed! ;)
yeah, the shit is strong. the first time
swijb touched it, about a 1/40 was tried. it was more than enough
for a 6 hour talk-fest.
i used the liquor trick too. turkey 101
and chard shoots...
the dosage is difficult. 99% of the
time, swijb would do waaay more than nessasary.
nothing exceeds like excess...
bu there seemed to be no ill effects
from too much, you would just stay fucked up forever.
i got in a fight with the lady b.i.t.d.,
and she was threatining to toss the prize rextaled .5 gram
super-pretty diamond chunky.
so i snatched it from the bitch and ate
it.
chomp, chomp, chomp. *gag* *choke*
i thought i was gonna die from the taste
alone. swijb chewed xtal like it was raw tang... it crunched like
sand. it made me salivate.. my mouth was burning after it started
disolving in my spit.
Swijb was fucked up for 3 days without
another dose.
Not always. Shaking salt with water doesnt
cause emulsions but the salt will dissolve considerably faster than
when not shaken. And many emulsions clear up fast.
Ever used a sep-funnel? Correctly, with shaking?
/fish
PS: Filtration through fine
glassfiber/cotton pads breaks virtually every emulsion.
Madness
takes its toll. Please have exact change
Edited
by - fishinabottle on Dec 30 2004 3:29:37 PM
Since the last 4-methylaminorex
postings, further improvements to the shake'n'bake method has been
discovered. The final missing milestone in the synthesis was the
lack of a decent salting procedure. None of the methods originally
devised by Eleusis / Zwitterion actually worked for making the
salt. Several bees have tried the method and all failed.
The only way of making a salt is by
adding equimolar amounts of hydrochloric acid, adding 10X xylol and
azeotropically distilling the water / xylol away. Xylol binds water
to a greater extent than toluene, which makes it more suitable for
drying stuff. After the solvent has been stripped, some acetone is
added and the whole mess cooled in the freezer. This will leave
glister white crystals of the hydrochloride in near quantitative
yields.
