反应详情

温度

-18 °C

50.12 g (154 mmol) is 8-acetyl-6-benzyloxy-2,2-dimethylbenzo[1,4]oxazin-3-one is reacted with selenium dioxide as oxidizing agent and activated charcoal in refluxing dioxane and some water. After cooling, the solid is filtered off and washed with dioxane. The filtrate is evaporated down and the residue is dissolved in 550 mL of ethanol and refluxed for 30 minutes. It is filtered and the mother liquor is cooled to −18° C., during which time a solid is precipitated which is suction filtered. After recrystallization from ethanol, the product is obtained in the form of a beige solid. Yield: 8.95 g (15%).

1. temperatureAfter cooling
2. filtrationthe solid is filtered off
3. washwashed with dioxane
4. customThe filtrate is evaporated down
5. dissolutionthe residue is dissolved in 550 mL of ethanol
6. temperaturerefluxed for 30 minutes
7. filtrationIt is filtered
8. customis precipitated which
9. filtrationfiltered
10. customAfter recrystallization from ethanol
11. customthe product is obtained in the form of a beige solid