反应详情

A 1 N sulfuric acid aqueous solution (30 ml) and 862.5 mg (12.5 mmol) of sodium nitrite were added at 0° C. to an acetic acid solution (15 ml) containing 1.52 g (5.0 mmol) of the 7-amino-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one obtained in Example 38. The obtained mixture was stirred for 30 minutes. Thereafter, 2.62 g (17.5 mmol) of sodium iodide and 952.3 mg (5.0 mmol) of copper iodide (I) were added to the reaction solution, and the obtained mixture was stirred at 80° C. for 1 hour. Thereafter, the reaction solution was cooled, and a saturated sodium bicarbonate aqueous solution was added thereto, followed by extraction with ethyl acetate. The extract was washed with a saturated saline solution, and was then dried over anhydrous sodium sulfate, followed by concentration. The obtained residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:4 to 1:2), and was then washed with a sodium thiosulfate aqueous solution, so as to obtain 1.87 g (90%) of 7-iodo-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one in the form of a light yellow solid.

1. stirringthe obtained mixture was stirred at 80° C. for 1 hour
2. temperatureThereafter, the reaction solution was cooled
3. extractionfollowed by extraction with ethyl acetate
4. washThe extract was washed with a saturated saline solution
5. dry with materialwas then dried over anhydrous sodium sulfate
6. concentrationfollowed by concentration
7. customThe obtained residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:4 to 1:2)
8. washwas then washed with a sodium thiosulfate aqueous solution