反应详情

To a solution of N-phenyl-benzene-1,2-diamine(3.08 g) in DMF (35 mL) was added potassium carbonate (2.31 g) and 2-bromo-N-isopropyl-N-(4-methoxy-phenyl)-acetamide (4.79 g) and stirred 18h at ambient temperature. The solvent was evaporated in vacuo and the resultant oil was dissolved in ethyl acetate(250 mL), washed with 1N HCl (4×100 mL), dried over sodium sulfate, filtered, and concentrated to a brown oil. The oil was subjected to flash chromatogaraphy on silica gel (70 g) eluted with ethyl acetate/hexanes (1:4, 1L). Fractions containing the desired product were combined and concentrated under reduced pressure to give the title compound as a tan foam (3.95 g).

1. customThe solvent was evaporated in vacuo
2. dissolutionthe resultant oil was dissolved in ethyl acetate(250 mL)
3. washwashed with 1N HCl (4×100 mL)
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated to a brown oil
7. washeluted with ethyl acetate/hexanes (1:4, 1L)
8. additionFractions containing the desired product
9. concentrationconcentrated under reduced pressure