HRID1353035
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
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
- temperaturethe reaction mixture was heated
- temperatureunder reflux for 2 h
- temperatureAfter cooling
- temperaturebriefly heated
- temperaturecooled again
- filtrationfiltered
- extractionIt was then extracted with dichloromethane
- dry with materialphase was dried (MgSO4)
- concentrationconcentrated