HRID1649845
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- extractionextracted with ethyl acetate (400 ml)
- dry with materialthe extract was dried over magnesium sulfate
- distillationThe solvent was distilled off
- custompurified by column chromatography on silica gel