反应详情

温度

110 °C

A suspension of 6-bromo-8-methoxyquinazolin-2-ol (43.96 mmol) in POCl3 (120 mL) was heated to 110° C. for 30 minutes The mixture was cooled to room temperature, evaporated POCl3 and partitioned between water and dichloromethane. The organic portion was concentrated to give a crude material which was purified by column chromatography (silica gel, eluted with 2% MeOH in dichloromethane) to yield pure material as a yellow solid in 30% yield (3 steps, 3.62 g). ES/MS m/z 272/274 (MH+).

1. temperaturewas cooled to room temperature
2. customevaporated POCl3
3. custompartitioned between water and dichloromethane
4. concentrationThe organic portion was concentrated
5. customto give a crude material which
6. customwas purified by column chromatography (silica gel, eluted with 2% MeOH in dichloromethane)
7. customto yield pure material as a yellow solid in 30% yield (3 steps, 3.62 g)