反应详情

温度

2.5 °C

A round-bottom flask under nitrogen atmosphere is loaded with N,N-diethyl-2-cyano-3-(-3-methoxy-4-hydroxy-5-nitrophenyl-)-acrylamide (134 g, 0.421 mol) dissolved in dichloromethane (0.65 l) and triethylamine (128 g, 1.26 mol). The solution is cooled to 0-5° C. and aluminium trichloride (67.4 g, 0.505 mol) is added in portions. After that, the mixture is refluxed for 3-4 hours, until completion of the conversion. The reaction mixture is cooled to 0-5° C., a 20% hydrochloric acid solution (0.5 l) is dropped in the mixture, which is left under stirring at room temperature for 30 minutes. The resulting solid is filtered, washing with water (0.1 l×3), and dried in a static dryer under reduced pressure at 50° C.; 126 g are obtained. Yield: 98%.

1. temperatureAfter that, the mixture is refluxed for 3-4 hours, until completion of the conversion
2. temperatureThe reaction mixture is cooled to 0-5° C.
3. waitis left
4. filtrationThe resulting solid is filtered
5. washwashing with water (0.1 l×3)
6. customdried in a static dryer under reduced pressure at 50° C.
7. custom126 g are obtained