反应详情

To a solution of methyl 4-(bromomethyl)-3-methoxybenzoate (250 mg, 0.965 mmol) in acetone (20.0 mL) were added potassium carbonate (267 mg, 1.93 mmol) and 5-chloro-6-isobutoxypyridin-3-ol (Preparation 1, 195 mg, 0.965 mmol) and the reaction mixture was heated at reflux for 16 hours, then allowed to cool to room temperature. The solvent was removed in vacuo to yield a yellow solid, which was partitioned between EtOAc (30.0 mL) and water (50.0 mL). The aqueous was further extracted with EtOAc (2×30 mL). The combined organics were washed with sodium hydroxide solution (1 M, 30 mL) then brine (50 mL), dried over sodium sulfate and the solvent was removed in vacuo to yield the title compound as a pale yellow solid.

1. temperaturethe reaction mixture was heated
2. temperatureat reflux for 16 hours
3. customThe solvent was removed in vacuo
4. customto yield a yellow solid, which
5. customwas partitioned between EtOAc (30.0 mL) and water (50.0 mL)
6. extractionThe aqueous was further extracted with EtOAc (2×30 mL)
7. washThe combined organics were washed with sodium hydroxide solution (1 M, 30 mL)
8. dry with materialbrine (50 mL), dried over sodium sulfate
9. customthe solvent was removed in vacuo