Reaktion #55018

Reaktionsgleichung

ethyl 4-[(4-chlorophenyl)amino]-1-piperidinecarboxylate

benzeneacetyl chloride

→

ethyl 4-[N-(4-chlorophenyl)-N-(phenylacetyl)amino]-1-piperidinecarboxylate

Lösungsmittel

benzene

benzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturrefluxed for 6h.15
2. 2
   TemperaturThe reaction mixture is cooled
3. 3
   Filtrationfiltered
4. 4
   WaschenThe filtrate is washed successively with water, sodium hydrogen carbonate solution and water
5. 5
   Sonstigedried
6. 6
   Sonstigeevaporated in vacuo
7. 7
   SonstigeThe residue is crystallized from 1,1'-oxybisethane

Vorschrift

To a stirred solution of 58 parts of ethyl 4-[(4-chlorophenyl)amino]-1-piperidinecarboxylate in 240 parts of benzene is added dropwise a solution of 46.2 parts of benzeneacetyl chloride in 80 parts of benzene at a temperature between 40°-70° C. Upon completion, the whole is stirred and refluxed for 6h.15. The reaction mixture is cooled and filtered. The filtrate is washed successively with water, sodium hydrogen carbonate solution and water, then dried and evaporated in vacuo. The residue is crystallized from 1,1'-oxybisethane, yielding 47 parts of ethyl 4-[N-(4-chlorophenyl)-N-(phenylacetyl)amino]-1-piperidinecarboxylate; mp. 108° C.

Quelle