HRID737114

反应详情

EQUATION

反应方程式

HRID 737114 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

100 mg of 3-phenyl-1-(2′-trifluoromethyl-biphenyl-4-ylmethyl)-piperazine was dissolved in a 2:1 mixture of dichloroethane and acetone, 2 equiv. of sodium triacetoxyborohydride was added followed by 30 μL of acetic acid. The reaction was stirred at room temperature under nitrogen overnight. The reaction was diluted with 5 mL of dichloromethane. The reaction mixture was washed with 1M aqueous sodium hydroxide solution and brine, then dried over sodium sulfate, filtered and concentrated in vacuo. The crude residue was purified by column chromatography to afford the title compound. Yield 41% ES MS m/z 439.

WORKUP

后处理

  1. additionwas added
  2. washThe reaction mixture was washed with 1M aqueous sodium hydroxide solution and brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe crude residue was purified by column chromatography