反应详情

At room temperature, 30 g of N′-[(2,6-difluorophenyl)-imino-methyl]-hydrazinecarboxylic acid tert-butyl ester and 23.8 g of glyoxylic acid ethyl ester are stirred in 500 ml of toluene at 70° C. for 4 hours. The reaction mixture is then concentrated, 200 ml of formic acid are added and stirring is continued at room temperature for 5 hours. The reaction mixture is concentrated, and the residue is taken up in 300 ml of ethanol and boiled under reflux for 6 h. After concentration of the reaction mixture and recrystallisation from ethyl acetate there is obtained 3-(2,6-difluorophenyl)-[1,2,4]triazin-6(1H)-one having a melting point of 219-226° C.

1. concentrationThe reaction mixture is then concentrated
2. addition200 ml of formic acid are added
3. concentrationThe reaction mixture is concentrated
4. temperatureunder reflux for 6 h
5. customAfter concentration of the reaction mixture and recrystallisation from ethyl acetate