HRID1596214

反应详情

EQUATION

反应方程式

HRID 1596214 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

To a stirred solution of (S)-1-tert-butoxycarbonyl-2-methyl-3-oxo-4-benzylpiperazine (1.0 g) in tetrahydrofuran (15 ml) was added borane-dimethylsulfide complex (0.49 ml) at 0° C. under nitrogen atmosphere. After stirring at 45° C. for 1.5 hours, borane-dimethylsulfide complex (0.46 ml) was added and the reaction mixture was stirred at 45° C. for another 2 hours. After cooled to 0° C., the reaction mixture was quenched with methanol. After evaporation of the solvent, the residue was purified by flash column chromatography eluting with a mixture of ethyl acetate and n-hexane (1:8) to give (S)-1-tert-butoxycarbonyl-2-methyl-4-benzylpiperazine (934 mg).

WORKUP

后处理

  1. additionborane-dimethylsulfide complex (0.46 ml) was added
  2. stirringthe reaction mixture was stirred at 45° C. for another 2 hours
  3. temperatureAfter cooled to 0° C.
  4. customthe reaction mixture was quenched with methanol
  5. customAfter evaporation of the solvent
  6. customthe residue was purified by flash column chromatography
  7. washeluting with a mixture of ethyl acetate and n-hexane (1:8)