反应详情

温度

90 °C

A stirred mixture of 15.3 g (0.073 mole) of methyl 2,6-dichloroisonicotinate in 180 ml of trifluoroacetic acid was heated at 90° C. During a six hour period 34 ml of 30% hydrogen peroxide was added to the hot reaction mixture in four to five ml aliquots. After complete addition the reaction mixture was stirred at 90° C. for two hours. The solvent was distilled from the mixture under reduced pressure to leave a solid. The solid was triturated with water, and the mixture was then filtered. The filter cake was recrystallized from acetone to yield 8.75 g of methyl 2,6-dichloroisonicotinate N-oxide.

1. additionAfter complete addition the reaction mixture
2. distillationThe solvent was distilled from the mixture under reduced pressure
3. customto leave a solid
4. customThe solid was triturated with water
5. filtrationthe mixture was then filtered
6. customThe filter cake was recrystallized from acetone