Carbazole → 9-(4'-Bromo-4-biphenylyl)carbazole

Temperatur

155 °C

A mixture of carbazole (300 mg, 1.81 mmol), 4,4′-dibromobiphenyl (846 mg, 2.71 mmol), copper (344 mg, 5.43 mmol), 18-crown-6 (187 mg, 0.71 mmol), potassium carbonate (750 mg, 5.43 mmol), and anhydrous N,N-dimethylformamide (10 mL) was degassed for 30 minutes. The mixture was heated to 155° C. for 66 hours under argon. After cooling, the mixture was poured into DCM (400 mL) and the subsequent mixture was filtered. The filtrate was loaded on silica gel. A flash column (silica, 10% DCM in hexane) and reprecipitation in DCM/hexanes yielded 304 mg (42% yield) of pure product; confirmed by HNMR.

1. customwas degassed for 30 minutes
2. temperatureAfter cooling
3. additionthe mixture was poured into DCM (400 mL)
4. filtrationthe subsequent mixture was filtered
5. customA flash column (silica, 10% DCM in hexane) and reprecipitation in DCM/hexanes

ORD-Eintrag

ord-b734a9f63b7f44e785846a6ca4178a00

Quelldatensatz

uspto-grants-2015_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08927121B2