反应详情

温度

130 °C

The mixture of 4-bromo-2-fluoro-5-methylaniline (203 mg, 1.0 mmol), 4-(methylcarbamoyl)phenylboronic acid (179 mg, 1.0 mmol), 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (82 mg, 0.2 mmol), Pd2(dba)3 (91 mg, 0.1 mmol), and K3PO4 (424 mg, 2.0 mmol) in 5.0 mL of n-butanol is degassed and heated at 130° C. for 1 h. The reaction mixture is concentrated in vacuo. The crude product mixture is partitioned between EtOAc and brine, the collected organic extracts are dried (Na2SO4), concentrated and purified with silica gel chromatography (EtOAc/hexanes:1/4) to afford 4′-amino-5′-fluoro-N,2′-dimethylbiphenyl-4-carboxamide; ESMS m/z 259.1 (M+H+).

1. customis degassed
2. concentrationThe reaction mixture is concentrated in vacuo
3. customThe crude product mixture is partitioned between EtOAc and brine
4. dry with materialthe collected organic extracts are dried (Na2SO4)
5. concentrationconcentrated
6. custompurified with silica gel chromatography (EtOAc/hexanes:1/4)