反应详情

7-Bromo-4-hydroxy-isoquinoline-3-carboxylic acid ethyl ester (1.0 g, 3.37 mmol) was dissolved in dry dichloromethane (30 mL) and bis(2,4,6-trimethylpyridine)iodine(I) hexafluorophosphate (3.5 g, 6.754 mmol) was added in one portion as a solid. The solution was protected from light and permitted to stir overnight at room temperature. Upon completion, the reaction was quenched by addition of aqueous sodium thiosulfate (2.0 g in 50 mL of water. The layers were separated and the organic phase washed with 1M hydrochloric acid, brine and dried over anhydrous sodium sulfate. The crude material was purified by silica gel chromatography (3-15% ethyl acetate in hexanes) to provide the iodo-isoquinoline in 77% yield which was used immediately in the next step.

1. customUpon completion, the reaction was quenched by addition of aqueous sodium thiosulfate (2.0 g in 50 mL of water
2. customThe layers were separated
3. washthe organic phase washed with 1M hydrochloric acid, brine
4. dry with materialdried over anhydrous sodium sulfate
5. customThe crude material was purified by silica gel chromatography (3-15% ethyl acetate in hexanes)