反应详情

温度

90 °C

Methyl 4-bromo-2-chloro-5-fluorobenzoate (2.10 g; 7.85 mmol; 1 eq.), zinc cyanide (553.15 mg; 4.71 mmol), tris(dibenzylideneacetone)dipalladium(0) (57.52 mg; 0.06 mmol), 1,1′-bis(diphenylphosphino)ferrocene (69.64 mg; 0.13 mmol; 0.02 eq.), zinc (20.54 mg; 0.31 mmol; 0.04 eq.) and zinc acetate (57.62 mg; 0.31 mmol; 0.04 eq.) were put in dry DMF (21 mL). The reaction mixture was purged with N2 and then heated to 90° C. for 12 hours. The reaction mixture was cooled to RT, filtered over a pad of celite and washed with EtOAc. The organic phase was washed with water, brine, dried over MgSO4 and concentrated affording the title compound as a brown solid. It was purified by washing with EtOH affording the title compound as a beige solid used without further purification. 1H NMR (DMSO-d6, 300 MHz) δ 8.36-8.35 (m, 1H), 8-7.97 (m, 1H), 3.90 (s, 3H). HPLC (Method A) Rt 4.02 min (Purity: 92.5%).

1. customThe reaction mixture was purged with N2
2. temperatureThe reaction mixture was cooled to RT
3. filtrationfiltered over a pad of celite
4. washwashed with EtOAc
5. washThe organic phase was washed with water, brine
6. dry with materialdried over MgSO4
7. concentrationconcentrated