反应详情

温度

100 °C

A mixture of 1-(3-bromo-5-tert-butylphenyl)-1H-imidazole 7 (0.98 g, 3.50 mmol, 1.0 eq), 9-(4-tert-butylpyridin-2-yl)-9H-carbazol-2-ol 10 (1.11 g, 3.50 mmol, 1.0 eq), CuI (0.10 g, 0.53 mmol, 0.15 eq), picolinic acid (0.13 g, 1.05 mmol, 0.30 eq) and K3PO4 (1.78 g, 8.40 mmol, 2.4 eq) in DMSO (7 mL) was stirred at a temperature of 100° C. for four days under a nitrogen atmosphere, then cooled to ambient temperature. The solid was filtered off and washed with plenty of ethyl acetate. The filtrate was washed with water three times and then dried over sodium sulfate and filtered. The filtrate was concentrated under reduced pressure and the residue was purified through column chromatography on silica gel using hexane/ethyl acetate as an eluent to obtain the desired product as a brown sticky liquid (1.45 g in 81% yield).

1. temperaturecooled to ambient temperature
2. filtrationThe solid was filtered off
3. washwashed with plenty of ethyl acetate
4. washThe filtrate was washed with water three times
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationThe filtrate was concentrated under reduced pressure
8. customthe residue was purified through column chromatography on silica gel