反应详情

To the solution of 4-(trifluoromethyl)phenyl methoxymethyl ether (5 g) in anhydrous ether (50 ml) was gradually added dropwise 1.6M n-BuLi (16.7 ml) at room temperature. After stirring at room temperature for 2 hours, the solution of DMF (4.13 ml) in anhydrous ether (20 ml) was added dropwise over 30 minutes, and the solution was stirred for 1 hour. To the reaction solution was added water, and the ether layer was separated. The ether layer is was washed with water and saturated sodium chloride solution, and dried over anhydrous sodium sulfate, and the solvent was removed under reduced pressure. The resulting residue was purified by chromatography on a silica gel column (methylene chloride:hexane=1:1), to give the title compound (4.49 g; 79%).

1. stirringthe solution was stirred for 1 hour
2. customthe ether layer was separated
3. washThe ether layer is was washed with water and saturated sodium chloride solution
4. dry with materialdried over anhydrous sodium sulfate
5. customthe solvent was removed under reduced pressure
6. customThe resulting residue was purified by chromatography on a silica gel column (methylene chloride:hexane=1:1)