反应详情

The reaction of Example 1 (reaction scale: 10 mmol of bromophenyl pyrazole) was conducted with 0.15 mole % of Pd2(dba)3. After the reaction was judged to be essentially complete, the reaction mixture was neutralized with 1N aq. HCl to a pH of 7.0 to 7.5. After filtration, the crude solid was dissolved in acetone (25 mL/g of bromophenyl pyrazole starting material) at 55° C. TMT (0.05 equiv.) was added, and the mixture was stirred for 1 h while the temperature was allowed to decrease to 30° C. The resulting solution was filtered twice through a Darco zeta pad. The filtrate was concentrated by partial removal of the organic solvents. Recrystallization from acetone/water afforded 2′-(5-ethyl-3,4-diphenyl-1H-pyrazol-1-yl)-[1,1′]-biphenyl-3-ol containing 33 ppm of palladium.

1. filtrationAfter filtration
2. dissolutionthe crude solid was dissolved in acetone (25 mL/g of bromophenyl pyrazole starting material) at 55° C
3. additionTMT (0.05 equiv.) was added
4. customto decrease to 30° C
5. filtrationThe resulting solution was filtered twice through a Darco zeta pad
6. concentrationThe filtrate was concentrated by partial removal of the organic solvents
7. customRecrystallization from acetone/water