HRID1353033
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 (64.6 g) was added to a solution of ethyl 3-allyloxycarbonylamino-3-(3-nitrophenyl)-propionate from II.1c (18.8 g) in 245 ml of ethanol, and the reaction mixture was heated under reflux for 2 h. After cooling the solution, it 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. 10.9 g of product were obtained.
WORKUP
后处理
- temperaturethe reaction mixture was heated
- temperatureunder reflux for 2 h
- temperatureAfter cooling the solution, it
- temperaturebriefly heated
- temperaturecooled again
- filtrationfiltered
- extractionIt was then extracted with dichloromethane
- dry with materialphase was dried (MgSO4)
- concentrationconcentrated