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Author: Subject: P2P from recycled styrene?
clearly_not_atara
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[*] posted on 25-5-2015 at 18:35


Quote:
Benzaldehyde + Ethyl acetate + NaOH (tiny amount, e1cb) --> diketone


^the expected product of the first reaction is ethyl cinnamate, not pyruvoylbenzene. The aldehyde won't act as a nucleophile unless you convert it to a dithiolane.

[Edited on 26-5-2015 by clearly_not_atara]
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cmos6667
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[*] posted on 26-5-2015 at 10:06


ah, my bad, thanks for the info :)
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CuReUS
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[*] posted on 27-5-2015 at 03:06


Quote: Originally posted by cmos6667  
Entirely OTC-ish:
diketone + NaBH4 --> glycol

since when did NaBH4 become OTC

[Edited on 28-5-2015 by CuReUS]
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cmos6667
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[*] posted on 27-5-2015 at 13:41


Doesn't OTC mean you can get it without much hassle? You can get a kg of NaBH4 for 150£ on ebay.
And yes, I think so too.
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byko3y
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[*] posted on 27-5-2015 at 16:44


I'm not sure whether customs will be happy to see sodium borohydride in the declaration, but I agree that NaBH4 is much easier to obtain and is less watcher, than LiAlH4.
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cmos6667
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[*] posted on 28-5-2015 at 14:02


ok so what about legos? buy you some heliozimt, dissolve it in whatever ABS dissolves in, add say 2 or 3 molar equiv formic acid, reflux it for 6 hours, add methyl iodide, followed by NaOH, bam, racemic meth oil :D

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GrayGhost
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[*] posted on 28-5-2015 at 14:39


Styrene to P2P, it has several reactions and is not direct.
Other ways with several reactions , Styrene to Phenylacetamide to Phenylacetic Acid to P2P .

Styrene, ammonium hydroxide,sulfur,ethanol (reflux in autoclave) Chinese patent. ( Someone attemp this?)

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byko3y
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[*] posted on 28-5-2015 at 17:02


Willgerodt-Kindler with ammonia is an old well known reaction, but yes, it requires autoclave, and not everybody here has autoclave.
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GrayGhost
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[*] posted on 28-5-2015 at 17:33


Quote: Originally posted by byko3y  
Willgerodt-Kindler with ammonia is an old well known reaction, but yes, it requires autoclave, and not everybody here has autoclave.


I am tempting build a autoclave with old glass bottle of 10mm thick
with turn movement ( need agitation) in hot water bath. The problem is the tap, posibility use Teflon.

http://mla-s1-p.mlstatic.com/sifon-de-vidrio-soda-la-cecilia...

The vessel is old sifon de soda ( syphon of carbonatate water) .

[Edited on 29-5-2015 by GrayGhost]
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byko3y
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[*] posted on 28-5-2015 at 22:04


The answer is simple - do not use 100 years old method without modifications. Actually, Kindler modification is all about secondary amines, while the ammonia route is called simply WIlgerodt reaction.
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GrayGhost
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[*] posted on 29-5-2015 at 11:03


Quote: Originally posted by byko3y  
The answer is simple - do not use 100 years old method without modifications. Actually, Kindler modification is all about secondary amines, while the ammonia route is called simply WIlgerodt reaction.


Yes Sir, but original Willgerodt reaction take more of 20 hours:o
It is impractical for me.
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byko3y
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[*] posted on 30-5-2015 at 00:39


I just don't want to give you a complete answer, because you need to know more about this reaction before you can do it yourself due to possible hydrogen sulfide generation. It has really complex mechanism, but conditions and work up are much more easy. And you need no autoclave in fact.
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CuReUS
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[*] posted on 30-5-2015 at 02:49


Quote:
by the Chinese patent in the linked thread, practically no H2S is evolved unless in the hands of a fool.

nicodem said this on pg 2,so formation of H2S can be prevented.
I don't understand why people are going crazy trying to produce phenylacetic acid like this,when a UV catalysed,photo semi-benzilic rearrangement of chloracetophenone would give it to them
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byko3y
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[*] posted on 30-5-2015 at 03:34


Maybe because yield of Favorsii rearrangement of α-chloro-acetophenone is 25% in acetone, 50% in acetonitrile, and no reaction in alcohol (reduced back to acetophenone). But it works much better for activated aromatics.
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Templar
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[*] posted on 6-6-2015 at 20:40


Quote: Originally posted by rannyfash  
i hope you dont mind me dropping this here, it is somewhat unrelated to a small minority however you could repeat the kornblum oxidation to obtain p2p instead of the last step using NH3 resulting in the censored product




[Edited on 14-7-2012 by rannyfash]


I believe someone tried this is in a pressure reactor, substitution of the Br group with an anime by dry ammonia in a solvent, except it was for the methylenedioxy amphetamine version. Jon I think? Well I remember there being a big long 5pg+ thread on thevespiary of people trying it and saying it didnt work. Maybe the MD bridge was too fragile under high temp/pressure. But looking at the history of amphetamine synthesises going back to the 19th and 20th centuries it should work.

Its good that this thread didnt devolve into holier-than-thou chemists sitting on their righteous high horses. No one is being forced to take drugs, and that's if the chemist is manufacturing them in large scale quantities to sell. The war on drugs is a sham, and anyone who believes it is for the good of the people is a fool; an absolute pseudo intellectual, regardless of whatever university paper slip you have.

RE sourcing chemicals, borohydride and LAH can be easily (although at varying degrees of economy) sourced from china. Some countries, like NZ and australia, will simply confiscate any white powders they come across regardless of whether or not they test positive for illegal drugs. They can then demand money for testing for YOU to prove YOUR innocence, 500-1000$. I do not know if other larger countries can get away with this (looking at you america) because it is illegal for the state to do such a thing if the legal system has the onus to prove something is illegal.

Borohydride and then 10% Pd/C can be had relatively readily and cheaply from china. It can offer a higher yielding, cleaner, cheaper and less dangerous synthesis than using LAH. But obviously it does not have the same scope of application as LAH.

I had ~30g of 10% Pd/C locked in customs for 4 months until suddenly it turned up one day when the pricks realized that a black moist powder didn't have drugs mixed into it.

Until you have tried sourcing chemicals from china, you cannot say that borohydride, LAH etc are impossible to source. Dont go asking for acetic anhydride, p2p, piperonal etc though. China may be lax, but theyre not as lax as some people would like!

For smaller, specialized chemical amounts its best to try out eastern yurop/russian etc sellers on auction sites.

Amphetamines are marvelous for intelligent, disciplined people to use sometimes for performance enhancement. Good luck with the synth guys just my 2c.




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leom8888
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[*] posted on 31-10-2015 at 16:05


I want to say is that you are too cool
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Waffles SS
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[*] posted on 1-11-2015 at 08:50


Reaxys search of all possible ways for synthesis Phenylacetone (P2P)
(Please don use it for illegal purpose)

Attachment: P2P.pdf (1.9MB)
This file has been downloaded 2851 times

[Edited on 1-11-2015 by Waffles SS]
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