反应详情

温度

150 °C

To a solution of N-(4-bromo-3-fluoro-2-methylphenyl)acetamide (72B) (2.18 g, 8.86 mmol) in DMF (20 mL) was added CuCN (2.61 g, 29.1 mmol). The mixture was stirred at 150° C. for 12 h and was then poured into ice (50 g). After warming to rt, the product was extracted with EtOAc (3×50 mL). The combined organic layers were washed with brine, dried and concentrated. The residue was purified via flash chromatography eluting with a solution of 5% methanol in 95% of EtOAc/hexane (1:1) to provide the title compound (1.51 g) as a white solid. LCMS: m/z 193 [M+H]+

1. temperatureAfter warming to rt
2. extractionthe product was extracted with EtOAc (3×50 mL)
3. washThe combined organic layers were washed with brine
4. customdried
5. concentrationconcentrated
6. customThe residue was purified via flash chromatography
7. washeluting with a solution of 5% methanol in 95% of EtOAc/hexane (1:1)