反应详情

温度

5 °C

A mixture of 6-(((dimethylamino)ethyl)amino)-3-hydroxy-7H-indeno[2,1-c]quinoline-7-on obtained in example 3 (100 mg, 0.3 mmol), conc. sulfuric acid (1 ml) and nitric acid (1 ml) was stirred at 5° C. for 2 hours. The reaction mixture was poured into ice water, and a crystal precipitated was collected by filtration. The crystal obtained was purified by silica gel column chromatography (eluent; a lower layer of chloroform:methanol:water=9:3:1(v/v/v)) and crystallized from ethanol-diethylether to give 60 mg (yield: 52.9%) of title compound. The physicochemical properties thereof are shown in table 1.

1. customa crystal precipitated
2. filtrationwas collected by filtration
3. customThe crystal obtained
4. customwas purified by silica gel column chromatography (eluent
5. customa lower layer of chloroform:methanol:water=9:3:1(v/v/v)) and crystallized from ethanol-diethylether