HRID601665
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
Under nitrogen atmosphere, 60% sodium hydrogenate (18 mg) was added at 0° C. to 2 ml solution of dimethylformamide with 100 mg of 6-bromo-2H-isoquinoline-1-one, and the mixture was stirred for 30 min. Then, 0.03 ml of methyl iodide was added at 0° C., stirred at room temperature for 2 hours. Cold water was added to the reaction solution, extracted with chloroform. Chloroform layer was washed with saturated saline solution, dried with anhydrous sodium sulfate. After distilling out the solvents under reduced pressure, residues were separated and purified by preparative thin-layer chromatography (hexane/ethyl acetate=3/1) to obtain 24 mg of the above compound as a white solid.
WORKUP
后处理
- stirringstirred at room temperature for 2 hours
- extractionextracted with chloroform
- washChloroform layer was washed with saturated saline solution
- dry with materialdried with anhydrous sodium sulfate
- distillationAfter distilling out the solvents under reduced pressure, residues
- customwere separated
- custompurified by preparative thin-layer chromatography (hexane/ethyl acetate=3/1)