反应详情

温度

80 °C

Method 6—Step b A mixture of N-(2-Amino-5-methoxy-phenyl)-5-bromo-2-fluoro-benzamide (1.45 g, 4.28 mmol) in acetic acid (15 mL) was heated at 80° C. overnight. Solvent was removed under reduced pressure and the crude purified by precipitation from AcOEt (20 mL), dried, recovered with a mixture of dichloromethane (20 mL) and methanol (1 mL) and washed with saturated NaHCO3 solution (3×5 mL), the organic layer recovered by filtration through phase separator, and the solvent removed under reduced pressure to obtain 0.86 g of the title compound (63%).

1. customSolvent was removed under reduced pressure
2. customthe crude purified by precipitation from AcOEt (20 mL)
3. customdried
4. customrecovered with a mixture of dichloromethane (20 mL) and methanol (1 mL)
5. washwashed with saturated NaHCO3 solution (3×5 mL)
6. filtrationthe organic layer recovered by filtration through phase separator
7. customthe solvent removed under reduced pressure