反应详情

A mixture of cyclohexane (215 ml, 2.0 moles), t-butyl hydroperoxide, 70% aqueous (77.1 g, 0.6 moles), molybdenum trioxide (1.44 g, 0.01 moles) and 1-oxyl-2,2,6,6-tetramethyl-4-piperidone (34 g, 0.2 moles) is charged into a 500 ml flask equipped with a Barrett trap. The mixture is stirred at reflux (80° C.) for two hours until no more water is collected. Then, the mixture is filtered by gravity into a pressure bottle and molybdenum trioxide (1.44 g, 0.01 mole) is added. Subsequently, the mixture is heated under stirring to 105° C. (2.34 bar) and held for 5 hours, until the color changes from deep orange to pale yellow. The mixture is filtered and the clear solution is washed with 10% aqueous sodium sulfite (100 ml) and subsequently with water (2×50 ml). The obtained clear solution is dried over sodium sulfate and then concentrated to give 50 g of the desired material as a clear yellow oil (Mass spectrum: m/e=253)

1. additionis charged into a 500 ml flask
2. customequipped with a Barrett trap
3. customis collected
4. additionis added
5. temperatureSubsequently, the mixture is heated
6. stirringunder stirring to 105° C. (2.34 bar)
7. filtrationThe mixture is filtered
8. washthe clear solution is washed with 10% aqueous sodium sulfite (100 ml) and subsequently with water (2×50 ml)
9. dry with materialThe obtained clear solution is dried over sodium sulfate
10. concentrationconcentrated