HRID968468

反应详情

EQUATION

反应方程式

HRID 968468 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

64.6 g of tin-(II) chloride were added to a solution of 18.8 g of ethyl 3-{[(allyloxy)-carbonyl]-amino}-3-(3-nitrophenyl)-propanoate from Example II.2.c in 245 ml of ethanol, and the mixture was heated to reflux for 2 h. The reaction mixture was hydrolized with 300 ml of aqueous 2N sodium hydroxide solution, then filtered through silica gel, and the filtrate was washed with dichloromethane. The organic phase was dried over magnesium sulphate and concentrated to yield 13.1 g of a white solid.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 2 h
  3. filtrationfiltered through silica gel
  4. washthe filtrate was washed with dichloromethane
  5. dry with materialThe organic phase was dried over magnesium sulphate
  6. concentrationconcentrated