反应详情

温度

160 °C

A mixture of Intermediate 3 (80 mg, 0.22 mmol), 3-bromo-4-methylpyridine (1 eq, 38 mg, 0.22 mmol) and cesium carbonate (1.5 eq, 108 mg, 0.33 mmol) in a 3:1 mixture of 1,4-dioxan:water (4 ml) was degassed with argon for 5 minutes. Palladium acetate (2 mg, 0.01 mmol), followed by triphenylphosphine (12 mg, 0.04 mmol) were then added and the whole mixture stirred at 160° C. for 20 mins in a microwave reactor. The reaction mixture was allowed to cool and partitioned between ethyl acetate and water. The organic layer was separated and evaporated under reduced pressure. The resulting product was purified on a 5 g Isolute™ Flash silica-gel column, eluting from 0-40% ethyl acetate in petroleum ether to give the title compound as a yellow oil (38 mg, 52%).

1. customwater (4 ml) was degassed with argon for 5 minutes
2. additionwere then added
3. temperatureto cool
4. custompartitioned between ethyl acetate and water
5. customThe organic layer was separated
6. customevaporated under reduced pressure
7. customThe resulting product was purified on a 5 g Isolute™ Flash silica-gel column
8. washeluting from 0-40% ethyl acetate in petroleum ether