HRID409285
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-bromo-4-methoxy-8-phenoxy-isoquinoline-3-carboxylic acid methyl ester (1.02 g, 2.63 mmol), copper (I) cyanide (470 mg, 5.25 mmol) and anhydrous dimethylformamide (8.8 mL) was refluxed for ten minutes before it was cooled to room temperature quenched with water and ethyl acetate. The slurry was filtered. The organic layer was washed with water, brine, dried over anhydrous sodium sulfate, concentrated in vacuo and the residue was purified by flash column chromatography on silica gel with a gradient of ethyl acetate and hexanes to give the title compound as a yellow solid (727 mg): MS: (+) m/z 334.83 (M+1).
WORKUP
后处理
- temperaturewas refluxed for ten minutes before it
- customquenched with water and ethyl acetate
- filtrationThe slurry was filtered
- washThe organic layer was washed with water, brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated in vacuo
- customthe residue was purified by flash column chromatography on silica gel with a gradient of ethyl acetate and hexanes