HRID581202

反应详情

EQUATION

反应方程式

HRID 581202 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (3R)-3,4-dibenzylpiperazin-2-one (2.5 g; 9.0 mmol) in dry tetrahydrofuran (30 ml) was placed under an atmosphere of nitrogen and stirred on an ice-bath. Lithium aluminiumhydride (5.0 ml; 1.0M in tetrahydrofuran) was added dropwise during 15 minutes. The mixture was then heated at reflux temperature for 2 h and then allowed top cool. Another portion of lithium aluminiumhydride (4.0 ml; 1.0M in tetrahydrofuran) was added and the mixture was refluxed for 1 h. The mixture was allowed to cool and then quenched with water and a 4N sodium hydroxide solution. Ethyl acetate (50 ml) was added and the mixture was filtered. The solvent was evaporated in vacuo to give 2.0 g of (2R)-1,2-dibenzylpiperazine.

WORKUP

后处理

  1. temperatureThe mixture was then heated
  2. temperatureat reflux temperature for 2 h
  3. temperaturethe mixture was refluxed for 1 h
  4. temperatureto cool
  5. customquenched with water
  6. additionEthyl acetate (50 ml) was added
  7. filtrationthe mixture was filtered
  8. customThe solvent was evaporated in vacuo