HRID1618326

反应详情

EQUATION

反应方程式

HRID 1618326 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. filtrationwere filtered
  2. washwashed with 200 ml ethanol
  3. customFiltrate was evaporated under vacuum
  4. addition300 ml water was added to the residue
  5. customobtained
  6. extractionwas extracted with 2×250 ml EtOAC
  7. extractionThe organic extract
  8. washwas washed with brine
  9. dry with materialdried over sodium sulphate
  10. customevaporated