반응 #48544

반응 방정식

ethyl isonipecotate

3-chlorobenzoyl chloride

triethylamine

→

title compound

1-(3-Chloro-benzoyl)-piperidine-4-carboxylic acid ethyl ester

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   온도cooled to between 10 and 15° C
2. 2
   농축concentrated under reduced pressure
3. 3
   workup.ADDITIONThe residue was diluted with ether
4. 4
   세척the solution washed with 1N hydrochloric acid, sodium carbonate solution (×3) and brine
5. 5
   건조It was then dried over MgSO4
6. 6
   기타evaporated under reduced pressure

실험 절차

A solution of ethyl isonipecotate (27.6 g, 175 mmol) in dichloromethane (50 ml) was added dropwise over 10 minutes to a solution of 3-chlorobenzoyl chloride (20 ml, 160 mmol) and triethylamine (28 ml, 200 mmol) in dichloromethane (500 ml) cooled to between 10 and 15° C. The reaction was then stirred at room temperature for 3 hours and concentrated under reduced pressure. The residue was diluted with ether, the solution washed with 1N hydrochloric acid, sodium carbonate solution (×3) and brine. It was then dried over MgSO4 and evaporated under reduced pressure, to give the title compound as a solid, 44.49.

출처