反应详情

温度

120 °C

Potassium carbonate (3.21 g, 23.2 mmol) was added to a solution of methyl 3-hydroxy-5-{[phenylmethyl]oxy}benzoate (3.00 g, 11.6 mmol) in DMF (30 mL) followed by addition of 1-fluoro-4-(methylsulfonyl)benzene (2.02 g, 11.6 mmol) and the reaction was heated at 120° C. for 3 h. The solvent was then removed in vacuo and the residue was taken up in saturated aqueous sodium hydrogencarbonate (50 mL) and ethyl acetate (150 mL). The organic layer was separated, washed with 1M aqueous hydrochloric acid (50 mL) then dried (MgSO4), filtered and evaporated. Purification by column chromatography, eluting with 1:4 to 1:1 ethyl acetate:hexanes, afforded the title compound as a colourless oil (3.50 g, 73%).

1. customThe solvent was then removed in vacuo
2. customThe organic layer was separated
3. washwashed with 1M aqueous hydrochloric acid (50 mL)
4. dry with materialthen dried (MgSO4)
5. filtrationfiltered
6. customevaporated
7. customPurification by column chromatography
8. washeluting with 1:4 to 1:1 ethyl acetate