反应详情

Combine 2-(4-methoxy-phenyl)-5,6-dihydro-4H-thieno[2,3-c]pyridin-7-one (0.245 g, 0.943 mmol), toluene-4-sulfonic acid 4-bromo-2-methoxy-phenyl ester (0.404 g, 1.13 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (xantphos) (27.3 mg, 0.05 mmol), and Cs2CO3 (0.461 g, 1.41 mmol) in dioxane (25 mL). Purge the reaction vessel with nitrogen for 5 min, and then add Pd2(dba)3 (8.6 mg, 0.09 mmol). Reflux the reaction mixture and stir 16 h. Dilute with EtOAc (100 mL), wash with water (2×30 mL), dry with Na2SO4, filter and concentrate. Purify the crude material by chromatography, eluting with 30-50% EtOAc/hexanes to give 0.432 g (86%) of the title compound. LC-MS/ES m/z 536.0 [M+H]+.

1. customPurge the reaction vessel with nitrogen for 5 min
2. temperatureReflux the reaction mixture
3. washwash with water (2×30 mL)
4. dry with materialdry with Na2SO4
5. filtrationfilter
6. concentrationconcentrate
7. customPurify the crude material by chromatography
8. washeluting with 30-50% EtOAc/hexanes