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 mixture of 1-(6-chlorobenzothiazole-2-yl)piperidine-4-ylamine (335 mg), acetone (92 ul), acetic acid (0.1 mL) and methanol (3 mL) was stirred at room temperature for 5 minutes. To the reaction solution was added triacetoxy sodium boron hydride (332 mg). The mixture was stirred at room temperature for 16 hours. The reaction solution was concentrated under reduced pressure. Aqueous sodium hydrogencarbonate was added thereto and extracted with ethyl acetate. The organic layer was washed with water and brine, and dried over sodium sulphate. The solvent was evaporated under reduced pressure and the residue was purified by column chromatograph on silica gel to give the title compound (160 mg). Yield: 41%.
WORKUP
后处理
- stirringThe mixture was stirred at room temperature for 16 hours
- concentrationThe reaction solution was concentrated under reduced pressure
- additionAqueous sodium hydrogencarbonate was added
- extractionextracted with ethyl acetate
- washThe organic layer was washed with water and brine
- dry with materialdried over sodium sulphate
- customThe solvent was evaporated under reduced pressure
- customthe residue was purified by column chromatograph on silica gel