HRID567113

反应详情

EQUATION

反应方程式

HRID 567113 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The above 1-(4-trifluoromethoxyphenyl)-3,4-dihydro-isoquinoline (0.40 g, 1.4 mmol) was dissolved in methanol (20 mL) and sodium borohydride (0.08 g, 2.1 mmol) was added slowly. The reaction mixture was stirred at room temperature for 2.5 hours. The mixture was evaporated in vacuo, redissolved in 1 N NaOH (20 mL) and extracted with dichloromethane (50 mL). The organic phase was dried (MgSO4), filtered and evaporated in vacuo. The remaining oil (0.35 g) was purified by column chromatography on silica gel eluting with a mixture of dichloromethane and methanol (9:1). This afforded 0.56 g (56%) of the title compound.

WORKUP

后处理

  1. customThe mixture was evaporated in vacuo
  2. dissolutionredissolved in 1 N NaOH (20 mL)
  3. extractionextracted with dichloromethane (50 mL)
  4. dry with materialThe organic phase was dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated in vacuo
  7. customThe remaining oil (0.35 g) was purified by column chromatography on silica gel eluting with a mixture of dichloromethane and methanol (9:1)