HRID1064597
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
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
- customThe solvents were then evaporated under reduced pressure
- dissolutionthe residue dissolved in methanol (50 ml)
- temperatureThe mixture then heated at 50° C. for 1 h
- customThe solvents were then evaporated under reduced pressure
- customPurification
- filtrationwas by trituration with ethyl acetate and filtration