反应详情

温度

10 °C

In a second vessel, (Z)-2,5-dichloro-N′-hydroxy-4,6-dimethylnicotinimidamide (201.2 g, 1.24 eq) is suspended in 1,4-dioxane (720 mL, 4.5 vol) and the suspension is cooled to 10° C. The residue of example 3e in 1,4-dioxane is added slowly maintaining the temperature below 20° C. A clear orange solution is formed. After complete addition, the reaction mixture is stirred at 20° C. for 1 hour. Pyridine (483.7 mL, 8 eq) is then charged and the reaction mixture is heated slowly to 115° C. The mixture is stirred at 115° C. for 6 hours. The solution is then cooled to 20° C. Dioxane/pyridine is distilled off.

1. temperaturemaintaining the temperature below 20° C
2. customA clear orange solution is formed
3. additionAfter complete addition
4. temperaturethe reaction mixture is heated slowly to 115° C
5. stirringThe mixture is stirred at 115° C. for 6 hours
6. temperatureThe solution is then cooled to 20° C
7. distillationDioxane/pyridine is distilled off