反应详情

Tetrabutylammonium iodide (53 mg) was added to a solution of the compound obtained in Example 9 (2) above (217 mg) in tert-butyl methyl ether (4 ml) under nitrogen atmosphere at 0° C. 3,5-Bis(trifluoromethyl)benzyl bromide (164 mg) was added dropwise and the solution was stirred for 4.5 hours while the temperature was gradually raised from 0° C. to room temperature. To the reaction mixture, were added with 1N hydrochloric acid and ethyl acetate, 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 (silica gel; hexane:ethyl acetate=19:1→4:1) to give the titled compound (182 mg). MS (m/z): 833 [M+H]+.

1. temperaturewas gradually raised from 0° C. to room temperature
2. customthe organic layer was separated
3. washwashed with a saturated brine
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated in vacuo
6. customThe resulting residue was purified by column chromatography (silica gel; hexane:ethyl acetate=19:1→4:1)