反应详情

Zinc powder (0.63 g) was added portionwise to a solution of 4-[N-(1,7-dichloroisoquinolin-3-yl)-N-methylamino]phenol (2.82 g) in a mixture of acetic acid (135 ml) and water (15 ml). On completion of the addition the mixture was heated under reflux for a period of 1 hour and was then filtered to remove any residual zinc. The solvent was removed by distillation under reduced pressure to give an oil. The oil was purified by chromatography over silica gel (eluant dichloromethane/ethyl acetate; 90:10) to give 4-[N-(7-chloroisoquinolin-3-yl)-N-methylamino]phenol (1.0 g) as an orange solid mp 140° C.

1. additionOn completion of the addition the mixture
2. temperaturewas heated
3. temperatureunder reflux for a period of 1 hour
4. filtrationwas then filtered
5. customto remove any residual zinc
6. customThe solvent was removed by distillation under reduced pressure
7. customto give an oil
8. customThe oil was purified by chromatography over silica gel (eluant dichloromethane/ethyl acetate; 90:10)