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
28 g (64.57 mmole) 2-(acetylamino)-2-[2(4-octylphenyl)ethyl]propanedioic acid diethylester (=compound according to formula (III)) was added to 450 ml ethanol. A solution of 17.91 g calcium chloride in 125 ml water was added in one lot. 12.21 g (322.7 mmole) sodium borohydride was added to the reaction mixture at 0° C. in 1 hr 20 min. The reaction mixture was left overnight for stirring. 100 ml of 1 N HCl was added to neutralize the reaction mixture and inorganic solids were filtered and washed with 200 ml ethanol. Filtrate was evaporated under vacuum. 300 ml water was added to the residue obtained and was extracted with 2×250 ml EtOAC. The organic extract was washed with brine, dried over sodium sulphate and evaporated to give 23 g semisolid.
WORKUP
后处理
- filtrationwere filtered
- washwashed with 200 ml ethanol
- customFiltrate was evaporated under vacuum
- addition300 ml water was added to the residue
- customobtained
- extractionwas extracted with 2×250 ml EtOAC
- extractionThe organic extract
- washwas washed with brine
- dry with materialdried over sodium sulphate
- customevaporated