反应详情

A mixture of ethyl 2-bromoacetate (0.23 g), 4-[N-(1,7-dichloroisoquinolin-3-yl)-N-methylamino]phenol (0.40 g), anhydrous potassium carbonate (0.19 g) and methyl ethyl ketone was heated under reflux for 12 hrs. The mixture was cooled, diluted with dichloromethane, washed with water and dried over anhydrous magnesium sulfate. The solvent was evaporated to give an oil, which was purified by column chromatography over silica gel (eluant dichloromethane) to give ethyl 2-{4-[N-(1,7-dichloroisoquinolin-3-yl)-N-methylamino]phenoxy}acetate (0.52 g) as a yellow crystalline solid, mp 99° C.

1. temperaturewas heated
2. temperatureunder reflux for 12 hrs
3. temperatureThe mixture was cooled
4. washwashed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe solvent was evaporated
7. customto give an oil, which
8. customwas purified by column chromatography over silica gel (eluant dichloromethane)