December 23, 2024, 09:16:55 AM
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Topic: Make N-Phenethyl-4-piperidone from 4-piperidone, will this work?  (Read 4264 times)

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Offline guesswork

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N-alkylation of 4-piperidone can be done in PTC conditions - and no need to isolate your piperidone as free base. Add to one liter of acetonitrile 3 mole finely powdered potassium carbonate, then add 10 g of PTC catalyst - TBAB or TEBA, or just polyethylene glycol-400. Stir this suspension 15 min at 50-60°C, and then add in little portions your 4-piperidone hydrochloride, watching that the CO2 evolution wasn't too vigorous. Stir another hour at 50-60°C, and then add dropwise phenethylbromide, and stir 15-20 h at mild reflux. Then cool, and filter off inorganic salts - if filtration goes too slowly, add to suspension some (30-40 ml) saturated sodium sulphate solution, this makes the sticky precipitate granular and filterable. Yield almost quantitative (trust me), and no distillation needed - as result you have slightly yellow solid with mp 60°C.


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Offline Mr Peanut

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Re: Make N-Phenethyl-4-piperidone from 4-piperidone, will this work?
« Reply #1 on: January 03, 2009, 12:13:01 PM »
Nasty. Do not ingest (without judgment of any kind). Trust me on this.

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