HRID2093086

反应详情

EQUATION

反应方程式

HRID 2093086 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of a piperidone hydrochloride (1 eq) in dichloromethane was added Et3N (2.1 eq) at 0° C. and the reaction mixture was stirred for 15 min. A solution ethyl chloroformate (1.1 eq) in chloroform was added at 0° C. and reaction was continued at room temperature for 3 h Reaction was quenched with water and extracted with ethyl acetate, organic layer was separated, dried over anhydrous Na2SO4 and concentrated under reduced pressure to afford crude product, which, on purification by column chromatography afforded the desired ethyl 4-oxopiperidine-1-carboxylate.

WORKUP

后处理

  1. customreaction
  2. waitwas continued at room temperature for 3 h
  3. customReaction
  4. customwas quenched with water
  5. extractionextracted with ethyl acetate, organic layer
  6. customwas separated
  7. dry with materialdried over anhydrous Na2SO4
  8. concentrationconcentrated under reduced pressure
  9. customto afford crude product, which
  10. customon purification by column chromatography