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
To a solution of 6-bromo-1-oxo-4-phenyl-1,2-dihydroisoquinoline-3-carboxylic acid methyl ester (1.30 g) in dimethylformamide (20 ml) was added sodium hydride (oil, 216 mg), and the mixture was stirred at room temperature for 20 min. 3-Bromomethylbenzoic acid methyl ester (990 mg) was added and the mixture was stirred at room temperature for 5 hrs. The solvent was evaporated under reduced pressure and 1N hydrochloric acid was added, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine and dried by adding sodium sulfate. The solvent was evaporated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=19/1→4/1) to give the title compound (719 mg, 39%).
WORKUP
后处理
- stirringthe mixture was stirred at room temperature for 5 hrs
- customThe solvent was evaporated under reduced pressure and 1N hydrochloric acid
- additionwas added
- extractionthe mixture was extracted with ethyl acetate
- washThe extract was washed with saturated brine
- customdried
- additionby adding sodium sulfate
- customThe solvent was evaporated under reduced pressure
- customthe obtained residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=19/1→4/1)