HRID1596214
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
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
- additionborane-dimethylsulfide complex (0.46 ml) was added
- stirringthe reaction mixture was stirred at 45° C. for another 2 hours
- temperatureAfter cooled to 0° C.
- customthe reaction mixture was quenched with methanol
- customAfter evaporation of the solvent
- customthe residue was purified by flash column chromatography
- washeluting with a mixture of ethyl acetate and n-hexane (1:8)