反应详情

温度

40 °C

Under a nitrogen atmosphere a solution of N-[2-(dimethylamino)ethyl]hydrazine (0.805 g) in THF (10.75 mL) is added to a stirred suspension of 9-fluoro-6-(p-toluenesulfonyloxy)benzo[g]isoquinoline-5,10-dione-2-oxide of Preparative Example 21 (1.075 g) in THF (10.75 mL). After stirring for 2 h, the mixture is heated to 40° C. for 1 h. After cooling to room temperature the mixture is poured in water (150 mL) and the obtained suspension is stirred for 2 h. The precipitate is recovered by filtration and recrystallized from ethyl acetate/n-hexane to give 2-[2-(dimethylamino)ethyl)]-5-(p-toluenesulfonyloxy)isoquino[8,7,6-cd]indazole-6(2H)-one-9-oxide (0.31 g).

1. temperatureAfter cooling to room temperature the mixture
2. stirringthe obtained suspension is stirred for 2 h
3. filtrationThe precipitate is recovered by filtration
4. customrecrystallized from ethyl acetate/n-hexane