反应详情

To a solution of phenyl N-(4-(6-carbamoyl-7-methoxy-4-quinolyl)oxy-2-chlorophenyl)carbamate (described in WO02/32872; 17.5 g, 37.7 mmol) dissolved in N,N-dimethylformamide (350 mL), was added cyclopropylamine (6.53 mL, 94.25 mmol) under nitrogen atmosphere, and the mixture were stirred at room temperature overnight. The mixture was poured into water (1.75 L), and stirred. Precipitated crude crystals were filtered off, washed with water, and dried at 70° C. for 50 minutes. Ethanol (300 mL) was added to the crude crystals, the mixture was heated to reflux for about 30 minutes to dissolve the crystals, and gradually cooled to room temperature overnight while stirring. Precipitated crystals were filtered off, dried in vacuo, and dried at 70° C. for 8 hours to give crystals of the title compound (12.91 g, yield 80.2 %).

1. stirringstirred
2. customPrecipitated crude crystals
3. filtrationwere filtered off
4. washwashed with water
5. customdried at 70° C. for 50 minutes
6. additionEthanol (300 mL) was added to the crude crystals
7. temperaturethe mixture was heated
8. temperatureto reflux for about 30 minutes
9. dissolutionto dissolve the crystals
10. temperaturegradually cooled to room temperature overnight
11. stirringwhile stirring
12. customPrecipitated crystals
13. filtrationwere filtered off
14. customdried in vacuo
15. customdried at 70° C. for 8 hours