反应详情

2-bromo-4-methoxy-6-[3-(trifluoromethyl)phenoxy] pyridine (3.00 g, 0.0086 mol) was suspended in about 30 ml of diethyl ether. While cooling in a dry ice-acetone bath in an argon atmosphere, the obtained suspension was mixed with n-butyl lithium [5.9 ml (ca. 1.69M hexane solution), 0.0086×1.1 mol], and the obtained suspension was stirred for about 10 minutes. After replacing an interior of the reactor with a carbon dioxide gas, the solution was removed from the bath and stirred at room temperature for about one hour. The obtained reaction solution was mixed with about 10 ml of a 1N aqueous hydrochloric acid solution, distributed in ethyl acetate-water, and then washed with saturated brine. The organic phase separated from the solution was dried with anhydrous sodium sulfate, concentrated and purified by silica gel column chromatography (eluting solution: ethyl acetate/hexane), thereby obtaining an aimed product.

1. temperatureWhile cooling in a dry ice-acetone bath in an argon atmosphere
2. customthe solution was removed from the bath
3. stirringstirred at room temperature for about one hour
4. customThe obtained reaction solution
5. washwashed with saturated brine
6. customThe organic phase separated from the solution
7. dry with materialwas dried with anhydrous sodium sulfate
8. concentrationconcentrated
9. custompurified by silica gel column chromatography (eluting solution: ethyl acetate/hexane)