反应详情

温度

10 °C

In a 250 mL three-necked round-bottomed flask equipped with a thermometer, droppingbfunnel and a condensor, 11.62 g of 3-nitro-2-phenyl-pyridine is dissolved in 58.0 ml of dichloromethane. Then, 13.65 g of H2O2 urea adduct is added. Under cooling with an ice/water bath, 16.40 ml trifluoroacetic acid anhydride is added dropwise over 25 minutes (temperature below 12° C.). After stirring at 10° C. for 45 minutes, the cooling bath is removed and the mixture is stirred at an ambient temperature for 18 hours. Afterwards, 150 ml of water is added (pH about 1) and extraction is carried out with dichloromethane (3×100 ml). After washing the organic phase with 10% aqueous sodium sulfite solution, it is dried over Na2SO4. After purification by chromatography on a pad of silica gel (eluent: first dichloromethane, then ethyl acetate), 9.45 g of the title compound is obtained as a yellow-green solid (MP: 116-117° C.).

1. customIn a 250 mL three-necked round-bottomed flask equipped with a thermometer, droppingbfunnel
2. temperatureUnder cooling with an ice/water bath
3. customthe cooling bath is removed
4. stirringthe mixture is stirred at an ambient temperature for 18 hours
5. additionAfterwards, 150 ml of water is added
6. extraction(pH about 1) and extraction
7. washAfter washing the organic phase with 10% aqueous sodium sulfite solution, it
8. dry with materialis dried over Na2SO4
9. customAfter purification by chromatography on a pad of silica gel (eluent