反应详情

To a solution of methyl 2-hydroxy-5-iodobenzoate (15 g, 53.9 mmol) in acetone (200 ml) was added 1-(bromomethyl)-4-fluorobenzene (9.95 ml, 81 mmol), potassium carbonate (14.91 g, 108 mmol) and the mixture was refluxed overnight. The mixture was allowed to cool and then filtered to remove the potassium carbonate. The solid potassium carbonate was washed with acetone (100 ml). The organics were combined and evaporated under reduced pressure on a buchi to give a solid. The solid was taken up into ethyl acetate (500 ml) and the organic phase was washed with water (2×200 ml), dried (MgSO4) and evaporated under reduced pressure on a buchi. The solid obtained was recrystallised from cyclohexane to yield the title compound as a white solid. 18.2 g.

1. temperaturethe mixture was refluxed overnight
2. temperatureto cool
3. filtrationfiltered
4. customto remove the potassium carbonate
5. washThe solid potassium carbonate was washed with acetone (100 ml)
6. customevaporated under reduced pressure on a buchi
7. customto give a solid
8. washthe organic phase was washed with water (2×200 ml)
9. dry with materialdried (MgSO4)
10. customevaporated under reduced pressure on a buchi
11. customThe solid obtained
12. customwas recrystallised from cyclohexane