反应详情

温度

160 °C

1.33 g (4.7 mmol) of ethyl [2-cyano-1-(2,4-dichlorophenyl)ethenyl]carbamate (Example 128A) and 740 mg (4.7 mmol) of 2-morpholin-4-ylacetohydrazide are dissolved in NMP (6 ml) and stirred in a flask with a calcium chloride drying tube at an oil-bath temperature of 160° C. for 3 h. The reaction mixture is cooled to RT and ethyl acetate (100 ml) and water (50 ml) are added. The organic phase is separated off, dried with magnesium sulphate and concentrated. The residue is chromatographed on silica gel (mobile phase dichloromethane/methanol 100:1 to 50:1). 1.25 g (70% of theory) of the product are 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 dichloromethane/methanol 100:1 to 50:1)
6. custom1.25 g (70% of theory) of the product are obtained