反应详情

To 1.24 g (4.27 mmol) of 6,7,8-trifluoro-1,4-dihydro-1-(1-methylcyclopropyl)-4-oxo-3-quinolinecarboxylic acid in 10 ml of acetonitrile was added 0.77 (4.27 mmol) of 3-[(t-butoxycarbonyl)amino]pyrrolidine and 0.63 g (4.27 mmol) of 1,8-diazobicyclo[5.4.0]undec-7-ene. The mixture was refluxed for one hour, cooled, filtered, and the solids washed with ether. The solids were dissolved in 10 ml of acetic acid at 100° C. and 2 ml of 3N hydrochloric acid was added. This mixture was heated at 100° for four hours, concentrated, triturated with 2-propanol, and the solid filtered, washed with ether, and dried (24 hours, 80° C., 125 mmHg) to give 0.90 g of 7-(3-amino-1-pyrrolidinyl)-6,8-difluoro-1,4-dihydro-1-(1-methylcyclopropyl)-4-oxo-3-quinolinecarboxylic acid as the hydrochloride salt, mp >300° C.

1. temperatureThe mixture was refluxed for one hour
2. temperaturecooled
3. filtrationfiltered
4. washthe solids washed with ether
5. dissolutionThe solids were dissolved in 10 ml of acetic acid at 100° C.
6. addition2 ml of 3N hydrochloric acid was added
7. temperatureThis mixture was heated at 100° for four hours
8. concentrationconcentrated
9. customtriturated with 2-propanol
10. filtrationthe solid filtered
11. washwashed with ether
12. customdried (24 hours, 80° C., 125 mmHg)