反应详情

温度

5 °C

A slurry of 1.20 kg of ethyl 7-azido-1-cyclopropyl-6,8-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylate in 12 L of dimethylformamide was charged to a five gallon autoclave. After placing the vessel under nitrogen, a slurry of 76 g of 10% palladium-on-carbon in 700 ml of dimethylformamide was added. The mixture was hydrogenated at 49-50 p.s.i. and 600 r.p.m. for four hours. The reaction mixture was filtered and concentrated under aspirator pressure to give a thick but stirrable dark residue. Ethanol (3 L) was added and the suspension was briefly refluxed before allowing to cool. After cooling to 5° C., the product was collected, washed with 2×500 ml of cold ethanol and then dried at 65°-70° C. in vacuo overnight to give 962 g (86.7%) of product.

1. filtrationThe reaction mixture was filtered
2. concentrationconcentrated under aspirator pressure
3. customto give a thick but stirrable dark residue
4. temperaturethe suspension was briefly refluxed
5. temperatureto cool
6. customthe product was collected
7. washwashed with 2×500 ml of cold ethanol
8. customdried at 65°-70° C. in vacuo overnight