Water → HCID 178517472, compound

Participants

Reaction Conditions

Reaction Steps

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.

Provenance & Evidence