反应详情

1.0 g (0.0032 mol) of 4-methoxy-6-{3-(trifluoromethyl)phenoxy}-2-pyridine carboxamide was dissolved in a mixed solvent containing about 20 ml of benzene and about 10 ml of DMF, and the obtained solution was mixed with 0.14 g (ca. 60% in mineral oil; 0.0032×1.1 mol) of NaH, followed by treating the solution under reflux for several minutes. Thereafter, the resultant reaction solution was mixed with 0.61 g (0.0032×2.0 mol) of chloromethyl ethyl ether, followed by treating the solution under reflux for about 3 hours. The reaction solution was distributed in ethyl acetate-saturated sodium bicarbonate water and then washed with saturated brine. The organic phase of 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. additionby treating the solution
2. temperatureunder reflux for several minutes
3. customThereafter, the resultant reaction solution
4. additionby treating the solution
5. temperatureunder reflux for about 3 hours
6. washwashed with saturated brine
7. dry with materialThe organic phase of the solution was dried with anhydrous sodium sulfate
8. concentrationconcentrated
9. custompurified by silica gel column chromatography (eluting solution: ethyl acetate/hexane)