Check erowid - i submittet a report about
4-mar some time ago... Can't remember if it was under the name
bandil or not... It was after an examn anyways, which i also wrote
about. You should be able to find it that way!
Bandil.....I was wondering if this method of shake and bake can
be used on a different amino alcohol , i.e. Phenylalaninol, the
alcohol of Phenylalanine. Whereas the PPA, aka. norephedrine is a
secondary amino alcohol(benzylic alcohol), does it react any easier
on the Potassium Cyanate than a primary alcohol on C3, if not then in
theory it should also be possible to start with the above mentioned
amino alcohol and produce 4-methylaminorex aka. 4-MAR,
"ICE". ? or will it be something different since the bond
is with the O in the C3 position as opposed to C1 as in PPA.........java
.........4-MAR
what I propose would be the O on C3
making the same oxazolone type ring with NH2...............
It's
better to die on your feet, than live on your knees...............Emiliano
Zapata (UH)
Your "azeotropic
crystallization" really rocks, Bandil! But is xylene really
better? I thought its higher bp would make for less yield, due to
the fact that more of the freebase evaporates together with the
water at higher temps?
Also in SWIAs dreams, every trace of
impurities becomes yellowish/brown with this procedure if he heats
thing up too quickly or too much, so one would have to use very
clean (distilled?) freebase for xylene IMO.
And why do you make the HCl salt of
4-MAR? I thought it was the free base being smokable, melting at
40°C or something like that? Is it for purification reasons, or am
I wrong with my assumption of 4-MAR freebase being common for
smoking?
Any smoke/vaporization bio assay reports with
4-MAR will bee much appreciated.
Still don't know what to believe about
it's vaporizability and the legends about smokable "street
ice". Not a lot of reliable info exists on this topic.
Also, is it true that the standard
"tweak" effects (negative ones) relating to sleep
deprivation that one might commonly get from meth are absent with
4-MAR?
And what are 4-MAR's effects on the
libido/sexual stamina?
Edited
by - TrainPullConductor on Feb 02 2005 03:21:16 AM
from what boog can tell, the salt is
more stable than the freeb. the freeb batches we used to get would
get greasy real easy... you couldnt care any freeb in your sock or
the shit would goo.
the 4-MAR high is different than meth...
4-MAR is a norephedrine modulator(boog
is spellin that totally wrong), meaning it affects the up take of
norephedrine in the brain. Norephidrine regulates the bodies
reaction speed and logical thought processes. its the same chemical
that makes ADHD kids ADHD. the new drug stratera is a norephedrine
uptake inhibitor. it functions similar to an SSRI, only it affects
norephiedrine...
4-MAR doent cause
hallucinations(innormal doeses) like meth can... the high can be
classified as a smart drug high. reaction times are improved,
logical thought are extreemly organized, sleep( or lack there of)
doesnt affect performance... if your feeling sluggish, hit a 20th
and youll be good for a few hours.
4-MAR is probably one of the longest
acting methylated phenyyethlamine boog has ever tried... the first
dose he did was a 10th of a g... entirly too much. that blast
lasted 10 hours without a doubt. a good dosage for street sale is
closer to a 40th of a gram.
and yes the shit was xtyl clear... boog
had some rocks that weighted 7 grams... solid chunks/xtyls...
Boog Night
isn't a chemist, bUt He plays one on Wetdreams.ws!! Ask him how!
the freeb would vap easy as hell, but
the smoke had less flavor that the salt. it was hard to tell if you
got a big hit of the freeb.
the hcl hit harder, too. you could feel
the HCl in your lungs. boog cant be certian if one did actully get
higher from the salt, but the feelings that go along with a big hit
were absent with the freeb.
Boog Night
isn't a chemist, bUt He plays one on Wetdreams.ws!! Ask him how!
Hm. Seems as the hydrochloride is far more
stable than the freebase - maybe this is the reason for the
"better" rush from smoking HCl salt vs. "absence of
feelings" when smoking freebase (freebase degrades and is
therefore "weaker")...
After reading J Chem Soc, 850-854
(1952), I found ideas for 4-Methylaminorex (4-MAR, U4EUh)
syntheses, with or without the use of cyanogen bromide. All the examples below
relates to the reaction of ephedrine and pseudoephedrine to form
racemic 3,4-dimethylaminorex isomers, but the exactly same schemes
should apply to phenylpropanolamine (PPA) to give 4-MAR. The two routes
described are either the classic cyanogen bromide cyclization of PPA and
formation of the carbamyl (substituted urea) derivative of PPA,
followed by acid treatment.
Using the cyanogen bromide route, the
cis-form of 4-methylaminorex can be had from the phenylpropanolamine isomer
corresponding to pseudoephedrine (1S,2S)/(1R,2R) and the trans-form from
the phenylpropanolamine corresponding to ephedrine
(1R,2S)/(1S,2R). The cyanogen bromide procedures below aren't optimized,
addition of 3 equivalents of sodium acetate and doubling the amount of
cyanogen bromide would not produce a precipitation of ephedrine salts, thus
making the procedure more effective (see other syntheses of 4-MAR on my
site).
Using the "double racemic"
phenylpropanolamine (1RS,2RS) would give equal amounts of racemic cis- and
trans-4-methylaminorex. All the cis/trans isomers are active, as well as their
respective stereoisomers. The trans(4S,5S) is the most potent, with an
effective dose of 0.25 mg/kg (compared to dextroamphetamine
considered active at 0.4 mg/kg and d-meth at 0.2 mg/kg). The cis isomers are of
about 5 times lesser potency, but they are still pretty active, as they
are about equipotent to racemic amphetamine, and with a 2-3 times longer
duration.
Using the potassium cyanate route, it
should be noted that only the PPA corresponding to the pseudoephedrine stereoconfiguration
(1S,2S) or (1R,2R) can be transformed into
trans-4-MAR (no cis-4-MAR is being produced either), the PPA corresponding
to the ephedrine stereoconfiguration (1S,2R) or (1R,2S)
will on the same treatment form trans-4-methyl-5-phenyl-oxazolid-2-one
(which looks just like 4-MAR, but with a double bonded oxygen instead of
the NH2 in the 2-position. It is an amide rather than an amine, so it should
be removable using an acid-base extraction.
The byproduct amide
trans-4-methyl-5-phenyl-oxazolid-2-one can be isolated and catalytically hydrogenated at room
temperature in ethanol containing 5% triethylamine and 10 mol% Pd/C to
form (S)-amphetamine in 90% yield, Ref: Chem Eur J, 3(8) 1370 (1997), but
that is probably not particularly useful, but using the potassium cyanate
scheme on substituted ephedrines (like the 3,4-methylenedioxy variety)
would enable you to produce a stereoselective synthesis of (S)-MDMA,
the more active isomer, together with the 3,4-methylenedioxy-trans-4-MAR
for evaluation of its activity.
Experimental
N-carbamyl-(±)-pseudoephedrine
5g (±)-Pseudoephedrine hydrochloride (25
mmol) in 50ml methanol was added a solution of 2g potassium cyanate
(KOCN, 25 mmol) in 150ml methanol, and the solution was heated under reflux for
one hour. Potassium chloride was filtered off and the filtrate evaporated
to dryness. The residue was recrystallized from 20ml of ethyl
acetate to give 2.2g of the substituted urea as white plates, mp 140-141°C.
(±)-trans-3,4-Dimethylaminorex HCl
A solution of
N-carbamyl-(±)-pseudoephedrine (1.56g, 7.5 mmol) in 24ml water and 15ml 2N HCl was refluxed for
three hours, when the clear solution was cooled the
(±)-trans-3,4-Dimethylaminorex hydrochloride precipitated. This was purified by basifying
the solution, extracting it with benzene (can use any non-polar
solvent here), and the solvent evaporated and the freebase converted to
the hydrochloride by gassing with dry HCl in ether. Yield 1.9g, 84%, mp
225-229°C.
60ml of an etheral solution containing
3.5g (30 mmol) cyanogen bromide was added to 200ml of an etheral solution
containing 11g (±)-ephedrine (66 mmol), whereupon 8.1g of ephedrine
hydrobromide separated (50% based on ephedrine input, 33 mmol, mp 186-188°C)
and was filtered off and washed with ether. The filtrate was
concentrated to 25ml, and white needles (1.5g, mp 71-73°C) of
(±)-cis-3,4-Dimethylaminorex freebase precipitated. The filtrate was concentrated further,
and the residual oil treated with ethanolic hydrogen chloride. The product
was recrystallized from a mixture of 25ml CHCl3, 10 ml acetone and 5ml
ether yielding 4.2g of (±)-cis-3,4-Dimethylaminorex
hydrochloride, mp 215-217°C.
40 ml of an etheral solution of 1.75g
cyanogen bromide (16.5 mmol) was added to a solution of 5.5g
(±)-pseudoephedrine (33 mmol) in 100ml ether and 80ml benzene. In addition to
precipitated pseudoephedrine hydrochloride (3.9g),
(±)-cis-3,4-Dimethylaminorex hydrochloride (2.2g) was obtained upon treatment of the
residual oil after evaporation of the solvent with ethanolic hydrogen
chloride, mp 215-217°C, identical to the sample prepared above.
Does anyone know how long a drive it is from potassium cyanide to
potassium cyanate? If swib had some KCN, would this be a very
"involved" process?
According to Thorpe's Dictionary of
Applied Chemistry, potassium permagnate can oxidize potassium
cyanide to potassium cynate No further information is available presently,
perhaps references can bee found in the future
