反应详情

To a solution of N-{5-[(cyclopropylamino)carbonyl]-2-methylphenyl}-5-[(2-methylprop-2-en-1-yl)oxy]-2-nitrobenzamide (8.73 g) in methanol (250 ml) was added a saturated solution of copper acetate in water (80 ml). Sodium borohydride (4.3 g) was added portionwise and the mixture stirred for a further 1 hour at room temperature. Ethyl acetate (300 ml) was added and the mixture washed with aqueous sodium hydrogen carbonate (200 ml). The combined aqueous extracts were extracted with ethyl acetate (2×200 ml), the resulting organics washed with brine (100 ml) and dried (magnesium sulfate) and Concentrated to give the crude 2-amino-N-{5-[(cyclopropylamino)carbonyl]-2-methylphenyl}-5-[(2-methylprop-2-en-1-yl)oxy]benzamide (3.6 g) as an oil which was used directly in the next step.

1. washthe mixture washed with aqueous sodium hydrogen carbonate (200 ml)
2. extractionThe combined aqueous extracts were extracted with ethyl acetate (2×200 ml)
3. washthe resulting organics washed with brine (100 ml)
4. dry with materialdried (magnesium sulfate)
5. concentrationConcentrated