反应详情

温度

120 °C

To a solution of 3-(5-bromo-thiazolo[5,4-b]pyridin-2-ylmethoxy)-2,6-difluoro-benzamide (0.15 g, 0.37 mmol) in 5 ml of anhydrous DMF was added allyl tributyltin (0.26 ml, 0.86 mmol) and degassed the reaction mixture for the 10 minutes. Tetrakis(triphenylphosphine) palladium (0) (0.007 g, 0.0056 mmol) was then added and the reaction mixture was heated at 120° C. for 1 h under the nitrogen atmosphere. Then reaction mixture was cooled to room temperature added water (25 mL) and extracted the compound with ethyl acetate. The combined organic layers were dried over anhydrous Na2SO4, and evaporated to dryness under reduced pressure. The compound was purified by column chromatography on silica (100-200 M) using ethyl acetate/Hexane (60:40) as the eluent to provide the title compound (0.10 g, 75%).

1. customdegassed the reaction mixture for the 10 minutes
2. customThen reaction mixture
3. temperaturewas cooled to room temperature
4. extractionextracted the compound with ethyl acetate
5. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
6. customevaporated to dryness under reduced pressure
7. customThe compound was purified by column chromatography on silica (100-200 M)