反应详情

温度

160 °C

2.00 g (7.0 mmol) of ethyl [2-cyano-1-(4-trifluoromethylphenyl)ethenyl]carbamate (Example 129A) and 0.73 g (7.0 mmol) of hydrazino(oxo)acetic acid are dissolved in NMP (7 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, mixed with water (20 ml) and stirred for 20 min. 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 suspended in water in an ultrasonic bath for 10 min. and then stirred for 30 min. The solid is filtered off and dried. 0.97 g (38% of theory) of the product are obtained.

1. temperatureThe reaction mixture is cooled to RT
2. stirringstirred for 20 min
3. customthe organic phase is separated off
4. dry with materialdried with magnesium sulphate
5. concentrationconcentrated
6. waitThe residue is suspended in water in an ultrasonic bath for 10 min.
7. stirringstirred for 30 min
8. filtrationThe solid is filtered off
9. customdried
10. custom0.97 g (38% of theory) of the product are obtained