反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture was then heated
- temperatureat reflux temperature for 2 h
- temperaturethe mixture was refluxed for 1 h
- temperatureto cool
- customquenched with water
- additionEthyl acetate (50 ml) was added
- filtrationthe mixture was filtered
- customThe solvent was evaporated in vacuo