反应详情

温度

120 °C

Under nitrogen, N-(3-bromo-2,6-dimethylthieno[2,3-b]pyridin-4-yl)-3-chlorobenzenesulfonamide (Example 61) (100 mg, 0.232 mmol) was dissolved in 1,4-dioxane (1.5 mL) and water (0.7 mL). (5-Methyl-2-thienyl)boronic acid (49.3 mg, 0.347 mmol), tetrakis(triphenylphosphine)palladium(0) (26.8 mg, 0.023 mmol) and potassium carbonate (96 mg, 0.695 mmol) were added and the mixture heated in a microwave at 120° C. for 10 min (×2). Ethyl acetate (10 mL) was added and the mixture washed with water (2×5 mL). The organic layer was dried over MgSO4, filtered and the solvent removed in vacuo. The residue was purified by normal phase chromatography, eluting with a gradient of 0-30% ethyl acetate in cyclohexane and then further purified by MDAP (acidic conditions), to give the title compound (16 mg). LCMS (A) m/z: 449 [M+1]+, Rt 1.54 min (acidic).

1. washthe mixture washed with water (2×5 mL)
2. dry with materialThe organic layer was dried over MgSO4
3. filtrationfiltered
4. customthe solvent removed in vacuo
5. customThe residue was purified by normal phase chromatography
6. washeluting with a gradient of 0-30% ethyl acetate in cyclohexane
7. customfurther purified by MDAP (acidic conditions)