반응 #216260

반응 방정식

4-piperidone hydrochloride hydrate

4-chlorobenzoyl chloride

potassium carbonate

→

title compound

수율 74.6%

N-(4-Chlorobenzoyl)-4-piperidone

수율 74.6%

용매

tetrahydrofuran

water

반응 조건

후처리

1. 1
   workup.ADDITIONare added successively
2. 2
   기타The organic phase is then separated off
3. 3
   추출the aqueous phase is extracted twice more with ethyl acetate
4. 4
   기타dried
5. 5
   기타evaporated down
6. 6
   workup.DISSOLUTIONThe residue is dissolved in ethyl acetate
7. 7
   workup.ADDITIONthe solution is treated with petroleum ether

실험 절차

87.5 g of 4-chlorobenzoyl chloride and a solution of 276 g of potassium carbonate in 552 ml of water cooled to 5° C. are added successively with stirring to a suspension of 80.6 g of powdered 4-piperidone hydrochloride hydrate in 1 l of tetrahydrofuran. The mixture is stirred at ambient temperature for a further 45 minutes. The organic phase is then separated off, the aqueous phase is extracted twice more with ethyl acetate, and the organic phases are combined, dried and evaporated down. The residue is dissolved in ethyl acetate and the solution is treated with petroleum ether. 88.6 g of the title compound of melting point 61°-63° C. are obtained.

출처