反应详情

To 750 mg (1.62 mmol) of 2-(3-cyclopropoxy-4-difluoromethoxyphenyl)-1-(2-trimethylsilylethoxymethyl)-1,5-dihydropyrrolo[2,3-d]pyridazin-4-one obtained in Example 1-(a) were added 2.5 ml of tetrahydrofuran, 0.22 ml of ethylenediamine and 16.5 ml of tetrahydrofuran solution containing 1M tetrabutylammonium fluoride, and the mixture was refluxed for 48 hours. After completion of the reaction, water and hexane were added to the reaction mixture, precipitated solid was collected by filtration, and dried under reduced pressure. The obtained dried material was dissolved in ethanol, poured into water, and precipitated solid was collected by filtration. The obtained solid was washed with water, and dried under reduced pressure to obtain 459 mg of the title compound as a white solid. (Yield: 85%)

1. temperaturethe mixture was refluxed for 48 hours
2. additionwere added to the reaction mixture
3. customprecipitated solid
4. filtrationwas collected by filtration
5. customdried under reduced pressure
6. dissolutionThe obtained dried material was dissolved in ethanol
7. additionpoured into water
8. customprecipitated solid
9. filtrationwas collected by filtration
10. washThe obtained solid was washed with water
11. customdried under reduced pressure