反应详情

温度

100 °C

To a stirred solution of 5-fluoro-3-methoxy-2-nitro-phenol (2.0 g, 10.6 mmol) in dimethylsulfoxide (25 ml) is added morpholine (9.2 ml, 106 mmol) at room temperature. The resulting mixture is heated at 100° C. for 2 h. After completion of reaction (monitored by TLC), the mixture is diluted with water (40 ml) and the aqueous layer is extracted with ethyl acetate (3×30 ml). The combined organic layers are washed with water (30 ml), brine (20 ml), dried over sodium sulfate and concentrated in vacuo. The crude product is purified by flash column chromatography (45% ethyl acetate/hexane) to yield 3-methoxy-5-morpholin-4-yl-2-nitro-phenol (0.71 g, 2.78 mmol, 26%).

1. customAfter completion of reaction (monitored by TLC)
2. extractionthe aqueous layer is extracted with ethyl acetate (3×30 ml)
3. washThe combined organic layers are washed with water (30 ml), brine (20 ml)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customThe crude product is purified by flash column chromatography (45% ethyl acetate/hexane)