HRID1784695

反应详情

EQUATION

反应方程式

HRID 1784695 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of (S)-3-benzyl-2,5-dioxopiperazine (2.284 g, 11.18 mmol) in tetrahydrofuran (20 mL) was added borane-tetrahydrofuran complex (49 mL, 1.0 M solution in THF, 49 mmol) at room temperature. The resulting mixture was refluxed for several hours before it was quenched with methanol at 0° C. After concentration in vacuo, the residue was treated with 10% sodium hydroxide aqueous solution, which was extracted with dichloromethane thoroughly. The organic layer was washed with water, dried over anhydrous sodium sulfate, and concentrated in vacuo to afford white crystals, which were washed with ether to yield (S)-2-benzylpiperazine (795 mg, 40.3%).

WORKUP

后处理

  1. temperatureThe resulting mixture was refluxed for several hours before it
  2. customwas quenched with methanol at 0° C
  3. concentrationAfter concentration in vacuo
  4. additionthe residue was treated with 10% sodium hydroxide aqueous solution, which
  5. extractionwas extracted with dichloromethane thoroughly
  6. washThe organic layer was washed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated in vacuo
  9. customto afford white crystals, which
  10. washwere washed with ether