反应详情

温度

160 °C

500 mg (1.75 mmol) of ethyl [2-cyano-1-(2,4-dichlorophenyl)ethenyl]carbamate (Example 128A) and 182 mg (1.75 mmol) of hydrazino(oxo)acetic acid are dissolved in NMP (2 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 stirred with diethyl ether/dichloromethane, and the solid is filtered off and dried. 150 mg (31% 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. stirringThe residue is stirred with diethyl ether/dichloromethane
7. filtrationthe solid is filtered off
8. customdried
9. custom150 mg (31% of theory) of the product are obtained