反应详情

温度

80 °C

To a solution of methyl 4-chloro-3-nitrobenzoate (2.0 g, 9.28 mmol) in anhydrous NMP (5 ml) was added 2d (2.03 g, 9.28 mmol) and triethylamine (1.3 ml, 9.28 mmol). The mixture was heated with stirring to 80° C. overnight. The cooled solution was poured into ice-water (50 ml) and the resulting mixture was extracted with ethyl acetate (3×10 ml). The combined organic extracts were washed with water, dried over sodium sulfate and evaporated to dryness. The residue was triturated with petroleum ether to yield methyl 4-(3-(1-acetylpiperazin-4-yl)anilino)-3-nitrobenzoate (3.14 g, 85%) as red crystals.

1. temperatureThe mixture was heated
2. extractionthe resulting mixture was extracted with ethyl acetate (3×10 ml)
3. washThe combined organic extracts were washed with water
4. dry with materialdried over sodium sulfate
5. customevaporated to dryness
6. customThe residue was triturated with petroleum ether