HRID968469
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
3-Nitrophenylsulphonyl chloride was added at 0° C. to a solution of 11.6 g ethyl 3-{[(allyloxy)-carbonyl]-amino}-3-(3-aminophenyl)-propanoate from Example II.2.d in 110 ml of pyridine. After a reaction time of 2 h, the mixture was concentrated, 1 N hydrochloric acid was added, and the solution was extracted with dichloromethane. After drying the organic phase over magnesium sulphate, the solvent was removed and the crude product was purified by chromatography on silica gel (dichloromethane/methanol=40:1) to give 17.8 g of a solid.
WORKUP
后处理
- concentrationAfter a reaction time of 2 h, the mixture was concentrated
- addition1 N hydrochloric acid was added
- extractionthe solution was extracted with dichloromethane
- dry with materialAfter drying the organic phase over magnesium sulphate
- customthe solvent was removed
- customthe crude product was purified by chromatography on silica gel (dichloromethane/methanol=40:1)