反应详情

温度

160 °C

A mixture of ethyl 6-(benzenesulphonylmethyl)-3-bromo-2-methoxybenzoate (Intermediate 61, 0.332 g), potassium methyltrifluoro borate (0.0675 g), palladium chloride dppf adduct with DCM (0.066 g) and cesium carbonate (0.786 g) in THF (9 ml) and water (1 ml) was sealed in a microwave vial and degassed. The mixture was then heated in the microwave at 160° C. for 30 minutes. After cooling, the mixture was dried (MgSO4) and filtered through Celite, and the pad was washed with ethyl acetate. The filtrate was evaporated to dryness and the residue was purified by chromatography on silica, eluting with a mixture of ethyl acetate and cyclohexane with a gradient of 0-50% to give ethyl 6-(benzenesulphonylmethyl)-2-methoxy-3-methylbenzoate (0.05 g) as a colourless gum.

1. customwas sealed in a microwave vial and
2. customdegassed
3. temperatureAfter cooling
4. dry with materialthe mixture was dried (MgSO4)
5. filtrationfiltered through Celite
6. washthe pad was washed with ethyl acetate
7. customThe filtrate was evaporated to dryness
8. customthe residue was purified by chromatography on silica
9. washeluting with a mixture of ethyl acetate and cyclohexane with a gradient of 0-50%