反应详情

温度

160 °C

2.42 g (8.5 mmol) of ethyl {2-cyano-1-[4-(trifluoromethyl)phenyl]ethenyl}carbamate (Example 129A) and 1.09 g (8.5 mmol) of 2,2,2-trifluoroacetohydrazide are dissolved in NMP (10 ml) 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 ethyl acetate (150 ml) and water (100 ml) are added. The organic phase is separated off, dried with magnesium sulphate and concentrated. The residue is stirred with diethyl ether (25 ml), and the solid is filtered off and dried. 0.67 g (23% 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. stirringThe residue is stirred with diethyl ether (25 ml)
6. filtrationthe solid is filtered off
7. customdried
8. custom0.67 g (23% of theory) of the product is obtained