反应详情

A mixture of 4-[N-(7-fluoro-1-hydroxyisoquinolin-3-yl)-N-methylamino]phenol (2.08 g) and phosphorus oxychloride was heated under reflux for approximately 10 minutes at which stage a clear solution had been obtained. The mixture was cooled and poured into ice-water. The precipitated solid was collected and purified by column chromatography over silica gel (eluant dichloromethane/ethyl acetate; 90:10) to give 4-[N-(1-chloro-7-fluoroisoquinolin-3-yl)-N-methylamino]phenol (2.00 g) as a yellow crystalline solid mp 130° C.

1. temperaturewas heated
2. temperatureunder reflux for approximately 10 minutes at which stage a clear solution
3. customhad been obtained
4. temperatureThe mixture was cooled
5. customThe precipitated solid was collected
6. custompurified by column chromatography over silica gel (eluant dichloromethane/ethyl acetate; 90:10)