反应详情

温度

140 °C

A mixture of ethyl 6-(benzenesulphonylmethyl)-3-bromo-2-methoxybenzoate (Intermediate 61, 0.347 g), cyclopropyl boronic acid monohydrate (0.087 g), palladium chloride dppf adduct with DCM (0.07 g) and cesium carbonate (0.8 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 140° C. for 15 minutes. After cooling, the mixture was dried (MgSO4) and filtered through Celite. The filtrate was evaporated to dryness and the residue was purified by chromatography on silica, eluting with a mixture of t-butyl methyl ether and cyclohexane with a gradient from 0-60% to give ethyl 6-(benzenesulphonylmethyl)-3-cyclopropyl-2-methoxybenzoate (0.187 g) as a 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. customThe filtrate was evaporated to dryness
7. customthe residue was purified by chromatography on silica
8. washeluting with a mixture of t-butyl methyl ether and cyclohexane with a gradient from 0-60%