反应详情

Phosphorus oxychloride (50 ml) was added to 5.0 g of the 6,7-dimethoxy-2-hydroxyquinazoline synthesized in Referential Example 89. They were heated and reacted for 8 hours under reflux. After allowing the reaction mixture to cool down, phosphorus oxychloride was distilled off under reduced pressure and the residue was dissolved in dichloromethane. After washing the dichloromethane solution once with a saturated aqueous solution of sodium bicarbonate, once with water and then once with saturated saline, the solution was dried with anhydrous sodium sulfate. The solvent was distilled under reduced pressure and the residue was purified by column chromatography (silica gel; eluent: 50:1 mixed solvent of dichloromethane and methanol), thereby obtaining 2.1 g of the intended product as crystals (yield: 38%).

1. customsynthesized in Referential Example 89
2. temperatureThey were heated
3. customreacted for 8 hours
4. temperatureunder reflux
5. temperatureto cool down
6. distillationphosphorus oxychloride was distilled off under reduced pressure
7. dissolutionthe residue was dissolved in dichloromethane
8. washAfter washing the dichloromethane solution once with a saturated aqueous solution of sodium bicarbonate
9. dry with materialonce with water and then once with saturated saline, the solution was dried with anhydrous sodium sulfate
10. distillationThe solvent was distilled under reduced pressure
11. customthe residue was purified by column chromatography (silica gel; eluent: 50:1 mixed solvent of dichloromethane and methanol)