反应详情

温度

60 °C

A mixture of copper(I) iodide (117 mg, 0.613 mmol), dichloropalladium-triphenylphosphane (1:2) (215 mg, 0.306 mmol), 2,4-dichloropyrimidine (913 mg, 6.13 mmol), and 5-ethynyl-2-{[3-(trifluoromethyl)phenyl]oxy}benzonitrile (880 mg, 3.06 mmol) in a mixed solvents of TEA (18 mL, 129 mmol) and tetrahydrofuran (12 mL), was added triphenylphosphine (161 mg, 0.613 mmol) under Argon. The reaction mixture was stirred for 12 h at 60° C., filtered, washed with EA, concentrated. Purification via ISCO system (EtOAc=1:20 to 1:5) afforded the title compound as a brown solid. LC-MS (ESI): m/z 400 [M+H]+; 3.86 min (ret time).

1. filtrationfiltered
2. washwashed with EA
3. concentrationconcentrated
4. customPurification via ISCO system (EtOAc=1:20 to 1:5)