反应详情

To 283 mg (0.593 mmol) of 2-(3-cyclobutoxy-4-difluoromethoxyphenyl)-1-(2-trimethylsilylethoxymethyl)-1,5-dihydropyrrolo[2,3-d]pyridazin-4-one obtained in Example 31-(a) were added 1.6 ml of dichloromethane and 5 ml of acetonitrile, then, 167 mg of sodium hydrogencarbonate and 367 mg of anhydrous magnesium sulfate were added to the mixture, and the resulting mixture was stirred at room temperature for 30 minutes. Then, 3 ml of dichloromethane solution containing 267 mg of iodine chloride was added to the same, and the resulting mixture was further stirred at room temperature for 4 hours. After completion of the reaction, a filtrate obtained by removing insoluble material in the reaction suspension by filtration and a washed solution obtained by washing the filtered solid with ethyl acetate were combined and the combined solution was washed successively with 5% aqueous sodium thiosulfate solution and then with a saturated aqueous solution of sodium chloride. The organic layer after washing was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The obtained residue was applied to silica gel column chromatography (Eluent; hexane:ethyl acetate=9:1→0:1 (V/V)), and the fractions containing the desired compound were concentrated under reduced pressure to obtain 314 mg of the title compound as a pale yellowish foam. (Yield: 88%)

1. additionwas added to the same, and the resulting mixture
2. stirringwas further stirred at room temperature for 4 hours
3. customAfter completion of the reaction
4. customa filtrate obtained
5. customby removing insoluble material in the reaction suspension
6. filtrationby filtration
7. customa washed solution obtained
8. washby washing the filtered solid with ethyl acetate
9. washthe combined solution was washed successively with 5% aqueous sodium thiosulfate solution
10. washThe organic layer after washing
11. dry with materialwas dried over anhydrous magnesium sulfate
12. concentrationconcentrated under reduced pressure
13. additionthe fractions containing the desired compound
14. concentrationwere concentrated under reduced pressure