HRID1088633

反应详情

EQUATION

反应方程式

HRID 1088633 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of (2S,4R)-1-allyloxycarbonyl-4-hydoxy-2-methoxycarbonylpyrrolidine (10 g) in tetrahydrofuran (20 ml) and ethanol (30 ml) was added by portions sodium borohydride (3.30 g) with stirring at 25°-30° C., and the mixture was stirred at the same temperature for 4 hours. To the reaction mixture was added dropwise conc. hydrochloric acid (7.27 ml) with stirring at 0°-2° C. The resulting precipitates were filtered off and the filtrate was evaporated in vacuo. The resulting residue was dissolved in a mixture of tetrahydrofuran (20 ml), ethanol (20 ml) and saturated aqueous sodium chloride (50 ml). The organic layer was evaporated in vacuo to give (2S,4R)-1-allyloxycarbonyl-4-hydroxy-2-hydroxymethylpyrrolidine (9.48 g).

WORKUP

后处理

  1. stirringthe mixture was stirred at the same temperature for 4 hours
  2. stirringwith stirring at 0°-2° C
  3. customThe resulting precipitates
  4. filtrationwere filtered off
  5. customthe filtrate was evaporated in vacuo
  6. dissolutionThe resulting residue was dissolved in a mixture of tetrahydrofuran (20 ml), ethanol (20 ml) and saturated aqueous sodium chloride (50 ml)
  7. customThe organic layer was evaporated in vacuo