反应详情

温度

60 °C

5.0 g (24.6 millimoles) of 6-(p-aminophenyl)-4,5-dihydro-5-methyl-3(2H)-pyridazinone are dissolved in 100 ml of absolute tetrahydrofuran by stirring and heating to 60° C. The solution is allowed to cool to room temperature, 5.15 g (29.7 millimoles) of 2,2-dichlorocyclopropanecarboxylic acid chloride, dissolved in 10 ml of absolute tetrahydrofuran, are added dropwise and the mixture is then stirred for 6 hours under reflux. Thereafter it is concentrated to about 50 ml and the product is filtered off at 10° C., washed with water and recrystallized from dimethylformamide/water. 5.0 g (60% of theory) of 6-[p-(2,2-dichlorocyclopropylcarbonylamino)-phenyl]-4,5-dihydro-5-methyl-3(2H)-pyridazinone are obtained as colorless crystals, of melting point 252°-253° C.

1. temperatureto cool to room temperature
2. additionare added dropwise
3. stirringthe mixture is then stirred for 6 hours
4. temperatureunder reflux
5. concentrationThereafter it is concentrated to about 50 ml
6. filtrationthe product is filtered off at 10° C.
7. washwashed with water
8. customrecrystallized from dimethylformamide/water