HRID968469

反应详情

EQUATION

反应方程式

HRID 968469 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationAfter a reaction time of 2 h, the mixture was concentrated
  2. addition1 N hydrochloric acid was added
  3. extractionthe solution was extracted with dichloromethane
  4. dry with materialAfter drying the organic phase over magnesium sulphate
  5. customthe solvent was removed
  6. customthe crude product was purified by chromatography on silica gel (dichloromethane/methanol=40:1)