反应详情

温度

100 °C

18.0 g 6-(3-methoxy-4-n-propoxyphenyl)-3[2H]pyridazinone are suspended in 63.6 g phosphorus oxytrichloride. The mixture is stirred at 100° C. until a clear solution has formed and the evolution of HCl stops. The solution is cooled to about 50° C. and poured onto 1 kg of ice, while stirring constantly, whereupon a crystalline precipitate forms immediately, this being filtered off with suction and washed free from acid with water, dilute sodium bicarbonate solution and again with water. Drying in vacuo gives 19.1 g (98.8%) of the title compound of m.p. 129° C., and of m.p. 132° C. after crystallization from cyclohexane.

1. customhas formed
2. temperatureThe solution is cooled to about 50° C.
3. stirringwhile stirring constantly, whereupon a crystalline precipitate forms immediately
4. filtrationthis being filtered off with suction
5. washwashed free from acid with water, dilute sodium bicarbonate solution and again with water
6. customDrying in vacuo