HRID1064597

反应详情

EQUATION

反应方程式

HRID 1064597 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A solution of the product from step (i) (1 g) in 1,2-dichloroethane (10 ml) was treated with 1-chloroethyl chloroformate (0.44 ml). The mixture was heated at 80° C. for 16 h. The solvents were then evaporated under reduced pressure and the residue dissolved in methanol (50 ml). The mixture then heated at 50° C. for 1 h. The solvents were then evaporated under reduced pressure. Purification was by trituration with ethyl acetate and filtration to give the subtitle compound as a white solid. Yield: 0.85 g

WORKUP

后处理

  1. customThe solvents were then evaporated under reduced pressure
  2. dissolutionthe residue dissolved in methanol (50 ml)
  3. temperatureThe mixture then heated at 50° C. for 1 h
  4. customThe solvents were then evaporated under reduced pressure
  5. customPurification
  6. filtrationwas by trituration with ethyl acetate and filtration