Acetic Acid → HCID 66604388, compound

Participants

Reaction Steps

Ethyl 4-(3′,4′-dichloro-3-cyanobiphenyl-4-ylamino)benzoate (410 mg, 0.997 mmol), diacetoxypalladium (560 mg, 2.492 mmol) in glacial acetic acid (20 mL) in a microwave tube (20 mL) were heated in microwave reactors at 160° C. for 4 h. The reaction was cooled to room temperature. The catalyst was filtered off and solid was washed with acetic acid several times. The filtrate was concentrated under reduced pressure and the residue was co-evaporated with toluene (3×). The resulting residue was suspended in ethyl acetate. The solid was collected by filtration and air dried to afford 75.4 mg of ethyl 8-carbamoyl-6-(3,4-dichlorophenyl)-9H-carbazole-3-carboxylate. MS (ESI) m/z 425.1(M−H). 1H NMR (DMSO-d6) δ ppmH NMR (DMSO-d6) d ppm 11.87 (1H, s), 9.00 (2H, m), 8.41 (1H, br. s), 8.40 (1H, d, J=1.22 Hz), 8.30 (1H, d, J=2.14 Hz), 8.06 (1H, dd, J=8.55, 1.53 Hz), 8.01 (1H, dd, J=8.24, 2.14 Hz), 7.82 (1H, d, J=8.55 Hz), 7.78 (1H, d, J=8.55 Hz), 7.65 (1H, br. s.), 4.38 (2H, q, J=7.22 Hz), 1.39 (3H, t, J=7.17 Hz).

Provenance & Evidence