反应详情

温度

0 °C

The compound obtained in Example 21 (2) above (177 mg) was dissolved in tert-butyl methyl ether (3 ml) under nitrogen atmosphere and the solution was cooled to 0° C. Thereto were added tetrabutylammonium iodide (46 mg), potassium tert-butoxide (105 mg) and 3-Bromomethyl-5-trifluoromethyl-benzonitrile (124 mg), and the mixture was stirred for 2 hours. 1N HCl and ethyl acetate were added to the reaction mixture and the organic layer was separated, washed with a saturated brine, dried over magnesium sulfate and concentrated in vacuo. The resulting residue was purified by column chromatography (NH-silica gel; hexane:ethyl acetate=4:1→3:2) to give the titled compound (39 mg). MS (m/z): 749 [M+H]+.

1. customthe organic layer was separated
2. washwashed with a saturated brine
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated in vacuo
5. customThe resulting residue was purified by column chromatography (NH-silica gel; hexane:ethyl acetate=4:1→3:2)