HRID728280
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
A solution of ethyl 3-amino-3-[1-(4-chlorophenyl)-cyclobutyl]acrylate (90 g), sodium cyanoborohydride (36 g), ammonium acetate (27 g) and acetic acid (60 ml) in ethanol (1.5 litres) was allowed to stand at room temperature for 5 days and then concentrated to 600 ml and poured into water (2.5 litres). The aqueous solution was basified, extracted with ether and the ether extract back extracted with 2N hydrochloric acid. The acidic aqueous extract was cooled with ice, basified and extracted with ether and the extract dried and evaporated to give ethyl 3-amino-3-[1-(4-chlorophenyl)cyclobutyl]propanoate.
WORKUP
后处理
- concentrationconcentrated to 600 ml
- additionpoured into water (2.5 litres)
- extractionextracted with ether
- extractionthe ether extract back
- extractionextracted with 2N hydrochloric acid
- extractionThe acidic aqueous extract
- temperaturewas cooled with ice
- extractionextracted with ether
- customthe extract dried
- customevaporated