反応 #216260

反応方程式

4-piperidone hydrochloride hydrate

4-chlorobenzoyl chloride

potassium carbonate

→

title compound

収率 74.6%

N-(4-Chlorobenzoyl)-4-piperidone

収率 74.6%

溶媒

tetrahydrofuran

water

反応条件

後処理

1. 1
   workup.ADDITIONare added successively
2. 2
   その他The organic phase is then separated off
3. 3
   抽出the aqueous phase is extracted twice more with ethyl acetate
4. 4
   その他dried
5. 5
   その他evaporated down
6. 6
   workup.DISSOLUTIONThe residue is dissolved in ethyl acetate
7. 7
   workup.ADDITIONthe solution is treated with petroleum ether

実験手順

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.

出典