反应详情

A mixture of 3-methoxycarbonyl-5-nitrobenzoic acid (44 mmol), SOCl2 (40 mL) and DMF (1 mL) was heated to reflux for 2 hours. Then the excessive SOCl2 was removed under reduced pressure. The residue was dissolved in DCM (80 mL), and added with NH3.H2O (15 mL) dropwise after cooling by ice-water. After addition, it was continued to stir 5 min. The resulting mixture was filtrated to give methyl-3-carbamoyl-5-nitrobenzoate in 85% yield.

1. temperaturewas heated
2. temperatureto reflux for 2 hours
3. customThen the excessive SOCl2 was removed under reduced pressure
4. dissolutionThe residue was dissolved in DCM (80 mL)
5. additionadded with NH3.H2O (15 mL) dropwise
6. temperatureafter cooling by ice-water
7. additionAfter addition, it
8. filtrationThe resulting mixture was filtrated