反应详情

温度

160 °C

2.10 g (7.4 mmol) of ethyl [2-cyano-1-(2,4-dichlorophenyl)ethenyl]carbamate (Example 128A) and 0.95 g (7.4 mmol) of 2,2,2-trifluoroacetohydrazide are dissolved in NMP (10 ml) under argon and stirred in a flask with a calcium chloride drying tube at an oil-bath temperature of 160° C. for 4 h. The reaction mixture is cooled to RT, and water (20 ml) is added. Ethyl acetate (150 ml) and water (100 ml) are added, and the organic phase is separated off, dried with magnesium sulphate and concentrated. The residue is chromatographed on silica gel (mobile phase cyclohexane/ethyl acetate 4:1 to 1:1). 0.97 g (38% of theory) of the product is obtained.

1. temperatureThe reaction mixture is cooled to RT
2. customthe organic phase is separated off
3. dry with materialdried with magnesium sulphate
4. concentrationconcentrated
5. customThe residue is chromatographed on silica gel (mobile phase cyclohexane/ethyl acetate 4:1 to 1:1)
6. custom0.97 g (38% of theory) of the product is obtained