反应详情

A mixture of 1-(3-fluoro-5-iodophenylcarbamoyl)-5-methoxy-6-trifluoromethylindoline (D17, 0.31 g, 0.65 mmol), 4-methyl-3-pyridylboronic acid (88 mg, 0.65 mmol), tetrakis (triphenylphosphine) palladium (O) (23 mg, 0.02 mmol) and sodium carbonate (0.31 g, 3.0 mmol) in 1,2-dimethoxyethane (20 mL) and water (2 mL) was heated under reflux for 24 h, then cooled and poured into water. The aqueous mixture was extracted with dichloromethane/methanol, and the organic extract was washed with brine, dried and evaporated. The residue was chromatographed on silica gel eluted with 2-3% methanol/dichloromethane to give the title compound, which was recrystallised from dichloromethane/petrol (80 mg, 28%), Mp 191-5° C.

1. temperaturewas heated
2. temperatureunder reflux for 24 h
3. temperaturecooled
4. extractionThe aqueous mixture was extracted with dichloromethane/methanol
5. extractionthe organic extract
6. washwas washed with brine
7. customdried
8. customevaporated
9. customThe residue was chromatographed on silica gel
10. washeluted with 2-3% methanol/dichloromethane