反应详情

Reaction was carried out in the same manner as in Example 1-(b) except for using 184 mg (0.353 mmol) of 2-(3-cyclopropoxy-4-difluoromethoxyphenyl)-3-ethoxymethyl-1-(2-trimethylsilylethoxymethyl)-1,5-dihydropyrrolo[2,3-d]pyridazin-4-one obtained in Example 12-(a) in place of 2-(3-cyclopropoxy-4-difluoromethoxyphenyl)-1-(2-trimethylsilylethoxymethyl)-1,5-dihydropyrrolo[2,3-d]pyridazin-4-one. 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 water and then with a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. To the obtained concentrate was added a small amount of tetrahydrofuran to dissolve the concentrate, hexane was then added thereto, and the mixture was subjected to ultrasonic wave treatment whereby the precipitated solid was collected by filtration. The obtained solid was washed with water and dried under reduced pressure to obtain 52 mg of the title compound as a white solid. (Yield: 38%)

1. customReaction
2. additionwas added to the reaction mixture
3. extractionthe mixture was extracted with ethyl acetate
4. customThe organic layer after separation
5. washwas washed successively with water
6. dry with materialwith a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. concentrationTo the obtained concentrate
9. additionwas added a small amount of tetrahydrofuran
10. dissolutionto dissolve the concentrate, hexane
11. additionwas then added
12. filtrationwas collected by filtration
13. washThe obtained solid was washed with water
14. customdried under reduced pressure