反应详情

温度

190 °C

2.4 g (8.4 mmol) of ethyl {2-cyano-1-[4-(trifluoromethyl)phenyl]ethenyl}carbamate (Example 129A) and 1.34 g (8.4 mmol) of 2-morpholin-4-ylacetohydrazide are dissolved in NMP (12 ml) and stirred in a flask with a calcium chloride drying tube at an oil-bath temperature of 190° C. for 4 h. The reaction mixture is cooled to RT and ethyl acetate (150 ml) and water (100 ml) are added. The organic phase is washed with saturated sodium bicarbonate solution, separated off, dried with magnesium sulphate and concentrated. The residue is chromatographed on silica gel (mobile phase cyclohexane/ethyl acetate 10:1 to 1:1, then with dichloromethane/methanol 100:1). 850 mg (26% of theory) of the product are obtained.

1. temperatureThe reaction mixture is cooled to RT
2. washThe organic phase is washed with saturated sodium bicarbonate solution
3. customseparated off
4. dry with materialdried with magnesium sulphate
5. concentrationconcentrated
6. customThe residue is chromatographed on silica gel (mobile phase cyclohexane/ethyl acetate 10:1 to 1:1
7. custom850 mg (26% of theory) of the product are obtained