反应详情

温度

0 °C

Trifluoromethanesulphonic anhydride (0.55 ml, 3.3 mmol) was added to a stirred suspension of 4-(chloro-2-fluoroanilino)-7-hydroxy-6methoxyquinazoline (959 mg, 3 mmol), (prepared as described for the starting material in Example 2), in methylene chloride (2.2 ml) and pyridine (2.2 ml) under argon at 0° C. The reaction mixture was stirred for 1 hour at 0° C., allowed to warm to ambient temperature and stirred for a further 1.5 hours. The volatiles were removed by evaporation, the residue was dissolved in ethyl acetate, washed with dilute hydrochloric acid and brine, dried (MgSO4) and the solvent removed by evaporation. The residue was triturated with ether/petroleum ether to give 4-(4-chloro-2-fluoroanilino)-6-methoxy-7-(trifluoromethylsulphonyloxyquinazoline (270 mg, 60%) as a beige solid.

1. custom(prepared
2. customat 0° C
3. temperatureto warm to ambient temperature
4. stirringstirred for a further 1.5 hours
5. customThe volatiles were removed by evaporation
6. dissolutionthe residue was dissolved in ethyl acetate
7. washwashed with dilute hydrochloric acid and brine
8. dry with materialdried (MgSO4)
9. customthe solvent removed by evaporation
10. customThe residue was triturated with ether/petroleum ether