反应详情

2.57 g (5 08 m Mol) of 6-fluoro-1-(2,4-difluoro-phenyl)-1,4-dihydro-4-oxo-7-(5-benzyl-2,5-diazabicyclo(2.2.1)-hept-2-yl)quinoline-3-carboxylic acid was dissolved in 170 ml of absolute ethanol containing 18 g of HCl and to the solution was added 2.1 g 10% Pd/c and the resultant hydrogenated at 15 psi and 60° C. for 2 hrs. After filtration of the catalyst the volatiles were removed under reduced pressure. The resulting residue was taken up in 80 ml of water and the pH adjusted to 7. The resulting suspension was heated for 20 mins. at 60° C. After cooling the precipitated was filtered and recrystallized from DMF to give 1.53 g (69.5%) of product as a hydrate, mp 198° C.-204° C. dec.

1. filtrationAfter filtration of the catalyst the volatiles
2. customwere removed under reduced pressure
3. temperatureThe resulting suspension was heated for 20 mins
4. customat 60° C
5. temperatureAfter cooling the precipitated
6. filtrationwas filtered
7. customrecrystallized from DMF