dormouse (Member)
04-21-00 05:35
No 108465
      Elf needs mescaline info, badly! -Starblood  Bookmark   


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Author  Topic:   Elf needs mescaline info, badly! 
Starblood
unregistered   posted 08-06-98 12:21 PM           
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Well a friend of mine is writing a novel where one of the characters is an evil anarchist bent on destroying our beloved society with his power to make people's heads explode. He got this power by eating a bunch of mescaline.
So my friend is trying to do some research on mescaline to make the story believable, so could anyone point me towards any good mescaline syntheses?
thanks.


EllisDTripp
Member   posted 08-06-98 01:05 PM          
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MESCALINE;
3,4,5-TRIMETHOXYPHENETHYLAMINE
SYNTHESIS: A solution of 20 g 3,4,5-trimethoxybenzaldehyde, 40 mL nitromethane, and 20 mL
cyclohexylamine in 200 mL of acetic acid was heated on the steam bath for 1 h. The reaction
mixture was then diluted slowly and with good stirring, with 400 mL H2O, which allowed the
formation of a heavy yellow crystalline mass. This was removed by filtration, washed with H2O, and
sucked as dry as possible. Recrystallization from boiling MeOH (15 mL/g) yielded, after filtration
and air drying, beta-nitro-3,4,5-trimethoxystyrene as bright yellow crystals weighing 18.5 g. An
alternate synthesis was effective, using an excess of nitromethane as solvent as well as reagent, if the
amount of ammonium acetate catalysis was kept small. A solution of 20 g
3,4,5-trimethoxybenzaldehyde in 40 mL nitromethane containing 1 g anhydrous ammonium acetate
was heated on the steam bath for 4 h. The solvent was stripped under vacuum and the residual
yellow oil was dissolved in two volumes of hot MeOH, decanted from some insolubles, and allowed
to cool. The crystals formed are removed by filtration, washed with MeOH and air dried yielding
14.2 g. of bright yellow crystals of beta-nitro-3,4,5-trimethoxystyrene. The use of these proportions
but with 3.5 g ammonium acetate gave extensive side-reaction products even when worked up after
only 1.5 h heating. The yield of nitrostyrene was, in this latter case, unsatisfactory.

To a gently refluxing suspension of 2 g LAH in 200 mL Et2O, there was added 2.4 g
beta-nitro-3,4,5-trimethoxystyrene as a saturated Et2O solution by use of a Soxhlet extraction
condenser modified to allow the continuous return of condensed solvent through the thimble. After
the addition was complete, the refluxing conditions were maintained for another 48 h. After cooling
the reaction mixture, a total of 150 mL of 1.5 N H2SO4 was cautiously added, destroying the
excess hydride and untimately providing two clear phases. These were separated, and the aqueous
phase was washed once with 50 mL Et2O. There was then added 50 g potassium sodium tartrate,
followed by sufficient NaOH to bring the pH >9. This was then extracted with 3x75 mL CH2Cl2,
and the solvent from the pooled extracts was removed under vacuum. The residue was distilled at
120-130 C at 0.3 mm/Hg giving a white oil that was dissolved in 10 mL IPA and neutralized with
concentrated HCl. The white crystals that formed were diluted with 25 mL Et2O, removed by
filtration, and air dried to provide 2.1 g 3,4,5-trimethoxyphenethylamine hydrochloride (M) as
glistening white crystals. The sulfate salt formed spectacular crystals from water, but had a broad and
uncharacteristic mp.


Labrat
Member   posted 08-07-98 09:34 AM          
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Yep, that synth works definitely, it comes right out of PIHKAL! Lr/
 
Starblood
unregistered   posted 08-11-98 12:27 PM           
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Well our fictional character is too lazy to use LAH, as he does not like to mess with gasses to keep the water vapor out.
Would the substitution of NaBH4 work?
 
Rhodium
Administrator   posted 08-11-98 01:49 PM          
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It is not necessary to use protection gasses when working with LAH, and no, NaBH4 wouldn't work.
 
dreamer
Member   posted 08-11-98 02:10 PM          
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what about NaBH4 and Trimethylsilyl Chloride http://www.lycaeum.org/~rhodium/chemistry/pictures/tmscl-2.gif  ?
 
Rhodium
Administrator   posted 08-11-98 10:33 PM          
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Much better idea. Please report the results.
 
drone 342
Member   posted 08-11-98 10:49 PM          
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It sure ain't environmental, but a Zn amalgam -- heavy on the Hg, will do the job right. High yields, too. If you can dispose of the Hg ethically, I highly recommend this method. Seriously.
-drone #342


Starblood
unregistered   posted 08-12-98 02:22 PM           
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Hmm, well I was under the impression that LAH reacted explosively with water vapor in the air, besides our character does not have access to it.
But I am thinking that further research into the Zn amalgam (as the character has access to hazardous waste disposal) or the NaBH4 + other stuff method would give our character the info she needs.
Can anyone point me to refs which might suggest optimum reaction conditions/ mole ratios?
Thanks for pointing me in the right directions, if the story ever gets written, I will tell you guys how it turns out.
 
Rhodium
Administrator   posted 08-14-98 05:03 AM          
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Well, there is a theorethical risk of explosions when working with LAH, but in practice, this is not especially bad. Unpublished results by Rhodium et al (1997), showed that even suspending fine LAH dust in moist air didn't result in any spectacular reaction, and throwing approx 100mg of LAH dust into a bucket of water gave a reaction not unlike the same procedure made with a crushed effervescent aspirin tablet.
This is not written to encourage careless handling of LAH, just to show that LAH isn't as dangerous as nitroglycerin.


 
dwarfer
Member   posted 06-24-99 05:04 PM          
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With regards to my on line correspondent, Predator, with whom I was discussing my usual pressurized dreams:
Hi dude... I recently translated J. Prakt. Chemie (1930) electrochemical
reduction of 3,4,5-trimethoxy-betanitrostyrene to mescaline, and will post
it to a.d.c as soon as it becomes practical for me to do so. Some of the
materials (porcellain made to proprietary specifications) are not
available but adequate ceramics almost certainly exist for substitution,
notably sintered borosilicate with a pore size of about 20 microns.

> Good luck

You too.

<predator>

Subj: Electrocatalytic-hydrogenation of nitrostyrenes

This is a posting of a translation from p346 of Journal fur Praktiche
Chemi (Vol 137) from the year 1933. Authors K. H. Slotta and G. Szyszka,
pertaining to the electrolytic reduction of
3,4,5-trimethoxy-beta-nitrostyrene to Mescalin. Probably works on a lot of
Shulgin-type precursors too.

I have yet to scan in the diagram which puts the equipment into some sort
of configurational significance. If it happens that I never get around to
doing that, you have the reference and can probably look it up. The
picture doesn't need translation from German.

ccm = ml ... a cubic centimetre. Letters in brackets refer to parts of the
picture.

--------------------------------------------------------------------------
A) Equipment for electrolytic reduction

An anode cell (Z) - a porous cell of Haldenwanger porcellain - was placed
in a filter assembly of 500 ccm (F) volume. The anode had measurements of
75mm x 160mm with a 70mm wide glazed edge that prevented the drawing-up
and smearing of the liquid to be reduced.

To the anode cellwas added a solution of 25ccm concentrated sulfuric acid
in 175ccm water.The anode used was lead or carbon rod and was enclosed in
a tightly wound, glass spiral cooler. The water in this was conducted to
the outer container to help cool the inner tube. By regulating the cooling
water it was possible to keep the whole reduction solutionfor the first
six hours at 20 degrees Celsius. In the last hours the temperature was
allowed to rise to 40 degrees Celsius, to get a nearly quantitative course
of the reduction.

The outer container contained a cathode (K) - a lead sheet (200mm x 90mm x
2mm), which before each experiment was coated electrolytically using
diluted sulfuric acid, with lead superoxide.

B) Reduction

A solution of 30g 3,4,5-trimethoxy-beta-nitrostyrene in 100ccm glacial
acetic acid and 100ccm ethanol was mixed with 50ccm concentrated
hydrochloric acid and added to the cathode container. The anode cell was
filled with dilute sulfuric acid to the outer level of the cathode cell.
Now a current of 5 to 6 amps was passed through the equipment for 12
hours, so that the current density was about 3 amps.

After the finished reduction, the contents of the cathode cell was
filtered and dried under vacuum. The remainder was then dissolved in
300ccm water. Any remaining unchanged nitrostyrene was removed by twice
shaking it out with ethyl acetate. The ester in the solution was then
removed by shaking out once with diethyl ether.

The liquid thus obtained of chloride of mescaline was then put in a
separating funnel which had ether added. The amine was freed with a cold
concentrated solution of technical sodium hydroxide. The solution
obtained, after extracting four times with ether, was dried with calcium
carbonate and the amine precipitated with dry hydrochloric acid gas.

After twice dissolving in absolute, dry, denatured alcohol, completely
pure mescalin hydroxide was obtained as white leaf with a melting point of
184 degrees Celsius and a yield of 24g (77.3%)

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<predator>


 
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