反应详情

1-Cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carbonitrile (5.04 g) and 3-(tertbutyloxycarbonylamino)pyrrolidine (3.96 g) were combined in acetonitrile (48 ml). The mixture was heated to reflux at which point all the solids dissolved. After refluxing for 15-20 minutes a precipitate formed. Stirring was continued at reflux overnight (22 hours). Triethylamine (6 ml) was then added and refluxing continued another seven hours before cooling to room temperature. The solid was collected by filtration and then washed with acetonitrile (15 ml) followed by a solution of triethylamine (5 ml) in acetonitrile (5 ml). The solid was dried under vacuum at 50° C. to give 7-[3-(tert-butyloxycarbonylamino)pyrrolidin-1-yl]-1-cyclopropyl-6,8-difluoro-1,4-dihydro-4-oxoquinoline-3-carbonitrile (7.65 g, 93%), mp 249°-250° C. (dec).

1. temperatureThe mixture was heated
2. temperatureto reflux at which point all the solids
3. dissolutiondissolved
4. temperatureAfter refluxing for 15-20 minutes a precipitate
5. customformed
6. temperatureat reflux overnight (22 hours)
7. temperaturerefluxing
8. filtrationThe solid was collected by filtration
9. washwashed with acetonitrile (15 ml)
10. customThe solid was dried under vacuum at 50° C.