HRID1353035

反应详情

EQUATION

反应方程式

HRID 1353035 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Tin(II) chloride (39.7 g) was added to a solution of ethyl 3-allyloxycarbonylamino-3(3-[3-nitrophenylsulphonylamino]-phenyl)-propionate from II.1e (16.8 g) in 155 ml of ethanol and the reaction mixture was heated under reflux for 2 h. After cooling, the solution was adjusted to pH=7 using 2N NaOH, briefly heated, cooled again and filtered. It was then extracted with dichloromethane, and the org. phase was dried (MgSO4) and concentrated. 7.3 g of product were obtained.

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 2 h
  3. temperatureAfter cooling
  4. temperaturebriefly heated
  5. temperaturecooled again
  6. filtrationfiltered
  7. extractionIt was then extracted with dichloromethane
  8. dry with materialphase was dried (MgSO4)
  9. concentrationconcentrated