反应详情

温度

80 °C

A suspension of 1.9 g of 8-(3-dimethylamino-1-azetidinyl)-3-ethoxycarbonyl-7-fluoro-1-methyl-4-oxo1,4-dihydrobenzo[b][1,8]naphthyridine in 20 cm3 of ethanol and 19 cm3 of 0.5N aqueous potassium hydroxide is heated with stirring to a temperature in the region of 80° C. for 5 hours. After cooling to approximately 5° C., the reaction mixture is treated with 9.5 cm3 of N aqueous methane sulphonic acid solution. The insoluble matter is drained, washed with twice 10 cm3 of water and 3 times 25 cm3 of ethanol and recrystallized in 125 cm3 of dimethylformamide. 1.4 g of 8-(3-dimethylamino-1-azetidinyl)-7-fluoro-1-methyl-4-oxo-1,4-dihydrobenzo[b][1,8]naphthyridine-3-carboxylic acid are obtained in the form of a yellow solid, which decomposes at 312° C.

1. temperatureis heated
2. temperatureAfter cooling to approximately 5° C.
3. washwashed with twice 10 cm3 of water and 3 times 25 cm3 of ethanol
4. customrecrystallized in 125 cm3 of dimethylformamide