反应详情

温度

10 °C

46.8 g (0.3 mole) of methyl 1-methylcarbonyl-2-ethoxyvinyl ketone were added dropwise to a suspension of 48.1 g (0.02 mole) of 3-amino-2,5,6-trichlorobenzoic acid in 100 ml of toluene. The mixture was heated for 2 hours to 80° C and was then cooled to 10° C, and the precipitate was filtered off. After digesting with acetonitrile, 52 g (74% of theory) of 3-[2,2-bis-(methylcarbonyl)-vinylamino]-2,5,6-trichlorobenzoic acid were obtained in the form of colourless crystals of melting point 242°-244° C.

1. temperatureThe mixture was heated for 2 hours to 80° C
2. filtrationthe precipitate was filtered off