反应详情

温度

100 °C

Under an argon atmosphere, (9R)-4-chloro-2-(4-hydroxy-4-methylpentyloxy)-9-(trifluoromethyl)-9H-fluoren-9-ol (169 mg) was dissolved in 1,4-dioxane (1.5 ml), ethyl 2-methyl-2-[4-(4,4,5,5-tetramethyl[1,3,2]dioxaborolan-2-yl)-1H-pyrazol-1-yl]propionate (194 mg), water (0.5 ml), tripotassium phosphate (178 mg), palladium acetate (9 mg), and SPhos (33 mg) were added, and the mixture was stirred at 100° C. for 4.5 hr. The reaction mixture was cooled to room temperature, water was added, and the mixture was extracted with ethyl acetate (twice). The obtained organic layer was washed successively with water (twice) and saturated brine. The obtained organic layer was dried over anhydrous magnesium sulfate, the insoluble material was filtered off, and the solvent in the filtrate was evaporated. The obtained residue was purified by silica gel column chromatography (a mixture of hexane and ethyl acetate at a mixing ratio 1:1 (hexane:ethyl acetate) was used as an elution solvent) to give the title compound (218 mg).

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionthe mixture was extracted with ethyl acetate (twice)
3. washThe obtained organic layer was washed successively with water (twice) and saturated brine
4. dry with materialThe obtained organic layer was dried over anhydrous magnesium sulfate
5. filtrationthe insoluble material was filtered off
6. customthe solvent in the filtrate was evaporated
7. customThe obtained residue was purified by silica gel column chromatography (
8. additiona mixture of hexane and ethyl acetate at a mixing ratio 1:1 (hexane:ethyl acetate)