反应详情

Under a nitrogen atmosphere, 60 mg of sodium hydride (60% oil dispersion) was added to 10 ml of dry THF. A solution of 0.41 g of 2-(3-chloro-4-ethoxyphenyl)-3,3,3-trifluoropropanol and 1.43 g of 3-(4-fluorophenoxy)benzyl bromide in 10 ml of dry THF was then added with ice-cooling, and the reaction solution was stirred with ice-cooling for 1 hour and at room temperature for 12 hours. Thereafter, the reaction mixture was poured into dilute HCl-ice water and extracted twice with diethyl ether. The ether layers were combined, washed with saturated sodium chloride solution and dried over anhydrous magnesium sulfate. The solvent was removed under a reduced pressure, and the residue was subjected to column chromatography on silica gel [eluted with n-hexane/ethyl acetate (40:1) mixture] to obtain 255 mg of the desired compound.

1. temperaturecooling
2. extractionextracted twice with diethyl ether
3. washwashed with saturated sodium chloride solution
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe solvent was removed under a reduced pressure