反应详情

温度

70 °C

A suspension of 0.8 g of ethyl 9-fluoro-4-methyl-1-oxo-8-pyrrolidinyl-1,4-dihydrobenzo[f][1,7]naphthyridine-2-carboxylate in a mixture of 60 Cm3 of aqueous ethanol at 50% and 2.8 cm3 of a 1 N aqueous potassium hydroxide solution was heated, with stirring, for 2 hours at a temperature of 70° C. After concentration under reduced pressure (5.2 kPa) at 60° C., the residue was dissolved in 100 cm3 of water; the light insoluble material was removed by filtration. The solution obtained was neutralized with 2.8 cm3 of a 1 N aqueous hydrochloric acid solution. The insoluble material formed was dewatered, washed 3 times with 20 cm of water, twice with 15 cm3 of ethanol and dried under vacuum at 100° C. 0.65 g of 9-fluoro-4-methyl-1-oxo-8-pyrrolidinyl-1,4-dihydrobenzo[f][1,7]naphthyridine-2-carboxylic acid was obtained in the form of yellow crystals, which melted at 365° C.

1. temperaturewas heated
2. concentrationAfter concentration under reduced pressure (5.2 kPa) at 60° C.
3. dissolutionthe residue was dissolved in 100 cm3 of water
4. customthe light insoluble material was removed by filtration
5. customThe solution obtained
6. customThe insoluble material formed
7. washwashed 3 times with 20 cm of water
8. dry with materialtwice with 15 cm3 of ethanol and dried under vacuum at 100° C