反应详情

温度

60 °C

Treat a slurry of 1-chloro-4-nitro-isoquinoline (2.5 g, 12 mmol) in acetonitrile (100 mL) with solid piperazine (5.2 g, 60 mmol). Heat the resulting yellow mixture overnight at 60° C. After cooling to ambient temperature, partition the reaction mixture between ethyl acetate and a saturated aqueous sodium bicarbonate solution. Add MeOH, dichloromethane and ethyl acetate, and filter the entire mixture to give a bright yellow solid. (2.15 g, 69%; LCMS ES+ (m/z) 259 [M+H]).

1. temperatureAfter cooling to ambient temperature
2. custompartition the reaction mixture between ethyl acetate
3. filtrationAdd MeOH, dichloromethane and ethyl acetate, and filter the entire mixture
4. customto give a bright yellow solid