反应详情

温度

50 °C

The reaction of Example 1 (reaction scale: 10 mmol of bromophenyl pyrazole) was conducted with 0.5 mole % of Pd2(dba)3. After the reaction was judged to be essentially complete, 5N aqueous HCl (1.25 mL/g of bromophenyl pyrazole starting material) was added followed by THF (12.5 mL/g) and water (2.5 mL/g). The mixture was heated to 50° C. to dissolve the precipitates, then cooled to 25° C. and filtered twice through a Darco zeta pad. To the filtrate was added TMT (5 mol %). The mixture was stirred at ambient temperature for 14 h and filtered again four times through the same Darco zeta pad employed in the previous filtration. The THF was removed by evaporation, and water (2.5 mL/g) and ethanol (2.5 mL/g) were added to precipitate the product, affording 2′-(5-ethyl-3,4-diphenyl-1H-pyrazol-1-yl)-[1,1′]-biphenyl-3-ol containing 146 ppm of palladium.

1. dissolutionto dissolve the precipitates
2. temperaturecooled to 25° C.
3. filtrationfiltered twice through a Darco zeta pad
4. additionTo the filtrate was added TMT (5 mol %)
5. filtrationfiltered again four times through the same Darco zeta pad
6. filtrationemployed in the previous filtration
7. customThe THF was removed by evaporation, and water (2.5 mL/g) and ethanol (2.5 mL/g)
8. additionwere added
9. customto precipitate the product