反应详情

Selenium dioxide (6.70 g, 61.0 mmol) was added to a solution of 4-fluoroacetophenone (8.43 g, 61.0 mmol) in dioxane (100 mL) and water (3 mL), and the resulting mixture was heated at 55° C. until complete dissolution of selenium dioxide had occurred. The reaction mass was then refluxed for 5-6 hrs. After completion of the reaction (TLC), the mixture was filtered and the filtrate was concentrated in vacuo affording a viscous oil. Water (50 mL) was added and the resulting mixture was stirred for 12 hrs, after which time the solid was collected on a filter, washed with water (25 mL) and dried in vacuo, affording 4-fluorophenylglyoxal (6.60 g, 85%).

1. temperatureThe reaction mass was then refluxed for 5-6 hrs
2. customAfter completion of the reaction (TLC)
3. filtrationthe mixture was filtered
4. concentrationthe filtrate was concentrated in vacuo
5. customaffording a viscous oil
6. customafter which time the solid was collected on a filter
7. washwashed with water (25 mL)
8. customdried in vacuo