反应详情

To 65 ml of acetonitrile solution containing 7.0 g (18 mmol) of 1,5-bis(2-trimethylsilylethoxymethyl)-1,5-dihydropyrrolo[2,3-d]pyridazin-4-one obtained in Reference example 18-(a) were added 6.0 g (71 mmol) of sodium hydrogencarbonate and 12.4 g (103 mmol) of anhydrous magnesium sulfate under argon atmosphere, and the mixture was stirred at room temperature for 1 hour. Then, 4.0 g (36 mmol) of s-caprolactam and 35.5 ml (35.5 mmol) of dichloromethane solution containing 1M iodine chloride were added to the mixture, and the mixture was further stirred for 3 hours. After completion of the reaction, water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer after separation was washed successively with 5% aqueous sodium hydrogen sulfite solution and then a saturated aqueous solution of sodium chloride, 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=5:1 (V/V)), and the fractions containing the desired compound were concentrated under reduced pressure to obtain 7.3 g of the title compound as a brownish solid. (Yield: 79%)

1. additionwere added to the mixture
2. stirringthe mixture was further stirred for 3 hours
3. additionwas added to the reaction mixture
4. extractionthe mixture was extracted with ethyl acetate
5. customThe organic layer after separation
6. washwas washed successively with 5% aqueous sodium hydrogen sulfite solution
7. dry with materiala saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate
8. concentrationconcentrated under reduced pressure
9. additionthe fractions containing the desired compound
10. concentrationwere concentrated under reduced pressure