反应详情

温度

75 °C

Bis(triphenylphosphine) palladium (II) chloride (49 mg, 0.07 mmol) was added to a degassed, ambient temperature solution of 1-methyl-5-(tributylstannyl)-1H-pyrazole (259 mg, 0.70 mmol) and 2-(4-bromophenyl)-3-[4-(2,2-dimethylpropyl)-1-trityl-1H-imidazol-2-yl]-1,1-difluoropropan-2-ol (483 mg, 0.77 mmol) in tetrahydrofuran (15 mL). After stirring at 75° C. overnight, the reaction mixture was cooled and cesium fluoride (50% on celite) was added. After stirring vigorously at ambient temperature for 1 h, the reaction mixture was filtered, rinsing with ethyl acetate. The filtrate was washed with water, dried (magnesium sulfate), filtered and concentrated in vacuo. Chromatography over silica eluting with 0-100% ethyl acetate/hexane afforded 3-[4-(2,2-dimethylpropyl)-1-trityl-1H-imidazol-2-yl]-1,1-difluoro-2-[4-(1-methyl-1H-pyrazol-5-yl)phenyl]propan-2-ol.

1. temperaturethe reaction mixture was cooled
2. stirringAfter stirring vigorously at ambient temperature for 1 h
3. filtrationthe reaction mixture was filtered
4. washrinsing with ethyl acetate
5. washThe filtrate was washed with water
6. dry with materialdried (magnesium sulfate)
7. filtrationfiltered
8. concentrationconcentrated in vacuo