HRID1784695
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe resulting mixture was refluxed for several hours before it
- customwas quenched with methanol at 0° C
- concentrationAfter concentration in vacuo
- additionthe residue was treated with 10% sodium hydroxide aqueous solution, which
- extractionwas extracted with dichloromethane thoroughly
- washThe organic layer was washed with water
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated in vacuo
- customto afford white crystals, which
- washwere washed with ether