Pyrazole → 1-(4-bromophenyl)-1H-pyrazole

Temperatur

82 °C

Into a 100-mL round-bottom flask, which was purged and maintained with an inert atmosphere of nitrogen, was placed a mixture of 1-bromo-4-iodobenzene (2.82 g, 9.97 mmol), 1H-pyrazole (680 mg, 9.99 mmol), CuI (380 mg, 2.00 mmol), DMEDA (430 μL, 4.00 mmol, 0.40 equiv), Cs2CO3 (6.52 g, 20.00 mmol) an CH3CN (40 mL). The resulting mixture was stirred overnight at 82° C. After cooling to ambient temperature, the solids were removed by filtration and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography with ethyl acetate/petroleum ether (1:12) as the eluent to yield the title compound as a white solid (2.1 g, 94%).

1. customInto a 100-mL round-bottom flask, which was purged
2. temperaturemaintained with an inert atmosphere of nitrogen
3. temperatureAfter cooling to ambient temperature
4. customthe solids were removed by filtration
5. concentrationthe filtrate was concentrated under reduced pressure
6. customThe residue was purified by silica gel column chromatography with ethyl acetate/petroleum ether (1:12) as the eluent

ORD-Eintrag

ord-79947f4bba6a4c42af0fa5cabd864385

Quelldatensatz

uspto-grants-2016_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09428502B2