反应详情

温度

105 °C

To a solution of 3-amino-5-chloro-2-nitrobenzoate (71; 3.3 g, 14.35 mmol) in DMF (66 ml) was added morpholine (48; 7.12 g, 81.78 mmol) and K2CO3 (11.28 g, 81.78 mmol). The resulting reaction mixture was stirred at 105° C. for 4 h. It was then filtered, diluted with water (500 ml), and extracted with EtOAc. The combined organic layers were dried (Na2SO4) and concentrated under reduced pressure. Column chromatography afforded methyl 3-amino-5-morpholino-2-nitrobenzoate 72 (2.1 g, 52.1%) as a brown yellow solid.

1. customThe resulting reaction mixture
2. filtrationIt was then filtered
3. additiondiluted with water (500 ml)
4. extractionextracted with EtOAc
5. dry with materialThe combined organic layers were dried (Na2SO4)
6. concentrationconcentrated under reduced pressure