反应详情

温度

100 °C

To a solution of 4-bromo-1-methyl-2-nitrobenzene (225 mg, 1.04 mmol), morpholine (125 μL, 1.25 mmol), and cesium carbonate (474.4 mg, 1.46 mmol) in toluene, palladium diacetate (31.2 mg, 0.139 mmol) and 2-(di-t-butylphosphino)biphenyl (125 mg, 0.403 mmol) are added and stirred at 100° C. for 5 hours. After cooling, the mixture is filtered to remove insoluble material. The filtrate is poured into water and extracted with ethyl acetate twice. The organic layer is washed with water and then brine, dried over magnesium sulfate, and evaporated in vacuo. The residue is purified with silica gel column chromatography (n-hexane:ethyl acetate=5:1) to afford 4-(4-methyl-3-nitrophenyl)-morpholine as a yellow solid.

1. temperatureAfter cooling
2. filtrationthe mixture is filtered
3. customto remove insoluble material
4. additionThe filtrate is poured into water
5. extractionextracted with ethyl acetate twice
6. washThe organic layer is washed with water
7. dry with materialbrine, dried over magnesium sulfate
8. customevaporated in vacuo
9. customThe residue is purified with silica gel column chromatography (n-hexane:ethyl acetate=5:1)