反应详情

温度

50 °C

4-(6-Bromo-pyridin-3-yl)-morpholine (3.16 g), tris(dibenzylideneacetone)-dipalladium (806 mg), and 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (2.2 g) were dissolved in toluene (60 ml) and the mixture was stirred under nitrogen atmosphere at 50° C. for an hour. The reaction mixture was cooled to room temperature, thereto was added the compound obtained in Example 8 (1) dissolved in toluene (10 ml) and the mixture was stirred at room temperature for 15 minutes. The stirring was further continued at 50° C. overnight after addition of sodium tert-butoxide (1.86 g). Water 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 to give the titled compound. The resulting residue was purified by column chromatography (silica gel; hexane:ethyl acetate=4:1→3:2) to give the titled compound (1.1 g). MS (m/z): 407 [M+H]+.

1. temperatureThe reaction mixture was cooled to room temperature
2. stirringthe mixture was stirred at room temperature for 15 minutes
3. customthe organic layer was separated
4. washwashed with a saturated brine
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated in vacuo