反应详情

温度

150 °C

A mixture of 4-chloro-3-[3-(methyloxy)phenyl]thieno[2,3-b]pyridine (Description 43) (100 mg, 0.363 mmol), 3-chlorobenzensulfonamide (90 mg, 0.471 mmol), palladium(II) acetate (8.14 mg, 0.036 mmol), xantphos (42.0 mg, 0.073 mmol), and Cs2CO3 (236 mg, 0.725 mmol) in 1,4-dioxane (3.6 mL) was degassed with nitrogen for 5 min. The mixture was heated at 150° C. for 45 min in a microwave and then poured into water (50 mL) and extracted with DCM (30 mL×4). The organic layers were combined, washed with brine (50 mL), dried over MgSO4, filtered and evaporated in vacuo. The residue was purified by chromatography on silica, eluting with a gradient of 0-10% ethanol in toluene, followed by further purification by MDAP (basic conditions), to give the title compound (72 mg). LCMS (A) m/z: 431 [M+1]+, Rt 1.34 min (acidic).

1. customwas degassed with nitrogen for 5 min
2. additionpoured into water (50 mL)
3. extractionextracted with DCM (30 mL×4)
4. washwashed with brine (50 mL)
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customevaporated in vacuo
8. customThe residue was purified by chromatography on silica
9. washeluting with a gradient of 0-10% ethanol in toluene
10. customfollowed by further purification by MDAP (basic conditions)