反应详情

t-Butyl hydroperoxide (70%, 65.2 g, 507 mmol), methylcyclohexane (150 ml), and sodium chloride (10 g) are agitated in a separatory funnel. The organic layer is dried over magnesium sulfate. The t-butyl hydroperoxidemethylcyclohexane solution is mixed with 35.0 g (127 mmol) of 4-benzoyloxy-1-oxyl-2,2,6,6-tetramethylpiperidine, 2.0 g of molybdenum trioxide, and 50 ml of methylcyclohexane. The reaction mixture is heated at reflux for 5 hours, then cooled to room temperature, filtered, and concentrated at reduced pressure. The crude product is diluted with heptane and passed through a short column of silica gel with heptane as the eluent to afford, after evaporation of solvent, 42.4 g (89% yield) of a clear colorless oil.

1. dry with materialThe organic layer is dried over magnesium sulfate
2. temperatureThe reaction mixture is heated
3. temperatureat reflux for 5 hours
4. filtrationfiltered
5. concentrationconcentrated at reduced pressure
6. additionThe crude product is diluted with heptane
7. customto afford