反应详情

温度

50 °C

The product from Example 1C (0.7 g, 1.433 mmol) and 4-bromoaniline (2.54 g, 14.33 mmol) were suspended in DMF (6 mL) and stirred at 50° C. overnight. The resulting mixture was partitioned between ethyl acetate (100 mL) and water (50 mL). The organic phase was washed with 1N HCl (2×50 mL) followed by a brine wash then dried over MgSO4 filtered and concentrated. The crude product was purified by chromatography on silica gel using a solvent gradient of 2-50% ethyl acetate in hexane to give the title compound as a mixture of stereoisomers (74.4 mg, 11% yield).

1. customThe resulting mixture was partitioned between ethyl acetate (100 mL) and water (50 mL)
2. washThe organic phase was washed with 1N HCl (2×50 mL)
3. washwash
4. dry with materialthen dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude product was purified by chromatography on silica gel using a solvent gradient of 2-50% ethyl acetate in hexane