反应详情

温度

5 °C

Trifluoromethanesulphonic anhydride (338 mg, 1.2 mmol) was added to a suspension of 4-(4-chloro-2-fluorophenoxy)-7-hydroxy-6-methoxyquinazoline (320 mg, 1 mmol), (prepared as described for the starting material in Example 5), in methylene chloride (2 ml) containing pyridine (2 ml) cooled at 5° C. When the addition was complete, the mixture was left to warm to ambient temperature and stirred for 1 hour. After removal of the volatiles by evaporation, the residue was partitioned between ethyl acetate/ether and water. The organic layer was separated, washed with 0.5M hydrochloric acid, followed by water, brine, dried (MgSO4) and evaporated to give 4-(4-chloro-2-fluorophenoxy)-6-methoxy-7-(trifluoromethylsulphonyloxy)quinazoline (400 mg, 88%).

1. custom(prepared
2. additionWhen the addition
3. waitthe mixture was left
4. temperatureto warm to ambient temperature
5. customAfter removal of the volatiles
6. customby evaporation
7. customthe residue was partitioned between ethyl acetate/ether and water
8. customThe organic layer was separated
9. washwashed with 0.5M hydrochloric acid
10. dry with materialdried (MgSO4)
11. customevaporated