HRID1649845

反应详情

EQUATION

反应方程式

HRID 1649845 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred mixture of 2-amino-4-[4-(diphenylmethoxy)piperidinomethyl]thiazole (8.04 g) and pyridine (7.72 ml) in dry N,N-dimethylformamide (80 ml) was added slowly a solution of propionyl chloride (2.76 ml) in dichloromethane (2 ml) at a temperature below 5° C. After 30 minutes, the reaction mixture was poured into ice water (800 ml) and extracted with ethyl acetate (400 ml), and the extract was dried over magnesium sulfate. The solvent was distilled off and purified by column chromatography on silica gel to give 2-propionylamino-4-[4-(diphenylmethoxy)piperidinomethyl]thiazole (8.9 g).

WORKUP

后处理

  1. extractionextracted with ethyl acetate (400 ml)
  2. dry with materialthe extract was dried over magnesium sulfate
  3. distillationThe solvent was distilled off
  4. custompurified by column chromatography on silica gel