反应详情

温度

140 °C

Solid potassium hydroxide (71 mg, 1.2 mmol) and then 4-chloro-6,7-dimethoxyquinazoline (0.25 g, 1.1 mmol), (prepared as described for the starting material in Example 1), were added to a melt of 2,4-dihydroxytoluene (0.6 g, 4.8 mmol) at 140° C. The mixture was stirred at 140° C. for 15 minutes, then allowed to cool. The mixture was diluted with water, and acidified to pH4 then extracted with ethyl acetate. The organic layer was washed with brine, dried (MgSO4) and the solvent removed by evaporation. The crude product was first purified by flash chromatography eluting with petroleum ether/ethyl acetate (1/9) and then by absorption HPLC eluting with trichloromethane/acetonitrile (85/15) to give 6,7-dimethoxy-4-(3-hydroxy-4-methylphenoxy)quinazoline (116 mg, 34%).

1. temperatureto cool
2. extractionthen extracted with ethyl acetate
3. washThe organic layer was washed with brine
4. dry with materialdried (MgSO4)
5. customthe solvent removed by evaporation
6. customThe crude product was first purified by flash chromatography
7. washeluting with petroleum ether/ethyl acetate (1/9)
8. customby absorption HPLC
9. washeluting with trichloromethane/acetonitrile (85/15)