反应详情

温度

70 °C

A 350 ml three-necked round-bottomed flask equipped with a magnetic bar, a thermometer, a dropping funnel and a reflux condenser is charged with 3-methyl-5-nitro-pyridin-2-ol (23.1 g), and 1,2-dichloroethane (150 ml). Phosphorous oxide chloride (17 ml) is added dropwise. Into this mixture DMF (11.5 ml) is added dropwise at room temperature. The reaction mixture is heated at 70° C. under stirring for 0.5 hour. After cooling the mixture to ambient temperature, it is concentrated in vacuo at 50° C., to obtain a brown oily gum. Purification of this gum by flash chromatography over silica gel with hexane/ethyl acetate 7:3 (v:v) gives 23.34 g of the compound as a light yellow solid (MP: 40-42° C.).

1. customA 350 ml three-necked round-bottomed flask equipped with a magnetic bar
2. temperatureAfter cooling the mixture to ambient temperature
3. concentrationit is concentrated in vacuo at 50° C.
4. customto obtain a brown oily gum
5. customPurification of this gum by flash chromatography over silica gel with hexane/ethyl acetate 7:3 (v:v)