反应详情

温度

140 °C

A stirred mixture of 10.0 g of 4-acetamido-2,2,6,6-tetramethylpiperidine-1-oxyl, 16 ml of 70% aqueous tert-butylhydroperoxide and 0.67 g of molybdenum trioxide in 75 ml of cyclohexane is heated under reflux in a flask fitted with a Dean-Stark apparatus. After 6 ml of water is collected, the reaction mixture is transferred to a Fisher Porter apparatus and heated at 140° C. and 30 psi for 4 hours. The decolorized reaction mixture is filtered and the filtrate is washed with water, aqueous sodium sulfite, brine, dried (MgSO4) and concentrated to give 13.61 g of a white solid. Recrystallization from heptane affords 10.39 g of the title compound as a white crystalline solid, m.p. 140°-44° C.

1. temperatureis heated
2. temperatureunder reflux in a flask
3. customfitted with a Dean-Stark apparatus
4. customAfter 6 ml of water is collected
5. customThe decolorized reaction mixture
6. filtrationis filtered
7. washthe filtrate is washed with water, aqueous sodium sulfite, brine
8. dry with materialdried (MgSO4)
9. concentrationconcentrated