反应详情

温度

80 °C

To a solution of EXAMPLE 106B (438 mg) and cyclohexanone (196 mg) in dioxane (3 ml) was added tris(dibenzylideneacetone)dipalladium(0) (5 mg), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (Xantphos, 7 mg) and Cs2CO3 (652 mg). The mixture was stirred at 80° C. under nitrogen overnight. After cooling, the reaction mixture was diluted with ethyl acetate and shaken with water. The product was extracted with ether (200 ml×3). The combined organic extracts were washed with water, brine, and dried over Na2SO4. After filtration, concentration of the mixture and flash column purification (3% ethyl acetate in hexane) provided EXAMPLE 106C.

1. temperatureAfter cooling
2. extractionThe product was extracted with ether (200 ml×3)
3. washThe combined organic extracts were washed with water, brine
4. dry with materialdried over Na2SO4
5. filtrationAfter filtration, concentration of the mixture and flash column purification (3% ethyl acetate in hexane)
6. customprovided EXAMPLE 106C