2-Oxo-PCE anyone have information on its synth?

psy

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Yes I have synthesized it before. Pain in my fucking ass is what it was. Started for cyclopentyl chloride, made the gringard, reacted it with benzaldehyde, oxidized it to the ketone with sodium dichromate, brominated it with elemental bromine, stirrered with excess KOH for 2 days to form the alcohol, added ethylamine with seives to remove the water, then microwaved it in decane, formed the salt, got high from it and wished I just bought a bag of ket instead of wasting 3 weeks. I had to do nearly every reaction twice because it failed the first time. This was years ago. Maybe I am better at chemistry now but I still hate it
 

IntrusiveReaction

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Is that the only way? isn't it a little doubtable that NL for example uses benzaldehyde when they are making O-PCE?
 

HerrHaber

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My imagination of the retrosynthetic analysis should also contain the more modern version for which I am quite sure that the 1-NO2-1-Ph-cyclohexa-2-one can be sourced. Then you reduce the nitro to amino and use an ethylating agent (not haloethane) rather diethyl sulfate and KOH a.q. where care must be taken not to Obtain the tertiary amine. As far as I observed the precursor market there is also the derivative with OH instead of NO2 and the one with alkene function instead of OH. I have never taken the ambition to perform such synthesis by the classic ciclopentane grignard as it is obvious why.
 

LazZzZz

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hello, i hope this finds you well, i recomend instead of starting from the very beggining, why not out source half the steps to China!!! id say look for a chemical called 2-phenylcyclohexanone, if you can then id reccomend buying as youll be 2 steps away from nedck. You can allwasy make this via grignards but again, please just purchase it lol. First you should disolve the 2-phenylcyclohexanone in a 50/50 mix of ethyl acetate and dcm and start to heat it up. Next, pour in a slurry of 2 mol equiv of CuBr2 and reflux for a couple of hours. Now remove the solvent using a rotovap or juss leave it next to a fan for a while and reduce it till a dry powder, perform a simple recrys for the bromo ketone however WATCH OUT. THIS IS A LACHRAMATOR!. After your new crystals have grown, time for the fun part. Dissolve 100 grams (0.348 mol) of your farm to table Bromoketone into 300cc of N-Methylpyriodine as your solvent. Add 132ml (1.74 mol) of 40% aqueous methylamine and leave stiring for 24 hours. Finally, pour numerous portions of toluene into the reaction mix and stir. Collect the organic phases and and salt out your final product. The best part is, this can make as many different ketalogues as youd like, stay safe and dont do this unless you know what youre doing. NMP is very toxic, the alpha-BromoKetone will cause hyou to cry if you get less than a miligram on your hands and you brush your face, trust me from experiance when i say it hurts
 
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HerrHaber

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This is a more relevant comment that is on the same line with what I was trying to say
 

12580

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G9zMmOeluo

怎么做这个?
 

testint

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I found this out in school fucking ouch
 

psy

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Yes you can buy more available precursors from china and I am sure it is way easier. I wasn't trying to produce it at any kind of scale and did it simply because I enjoy dissociatives. I designed a lot of the procedure myself. I think it is more common to use the nitrile instead of benzaledhyde but I did it all with chemicals I already owned.
 

testint

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I think I am cursed for getting the carbon carbon bond reaction to react every time I dare not speak it's name
 
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