反应详情

温度

140 °C

A two-phase mixture of 70% aqueous t-butyl hydroperoxide (103.9 g, 807 mmol), cyclohexane (200 ml) and sodium chloride (15 g) is shaken in a separatory funnel. The organic phase is dried over magnesium sulfate, filtered, and added to 40.0 g (101 mmol) of di-(2,2,6,6-tetramethylpiperidin-4-yl) succinate. Molybdenum oxide (2.0 g) is added, and the mixture is refluxed for one hour. Water is collected in a Dean-Stark trap. The entire reaction mixture is then transferred to a Fischer-Porter bottle and heated at 140° C. for 6 hours. Additional t-butyl hydroperoxide (90%, 10.1 g, 101 mmol) is added and heating is resumed for another 4 hours. The colorless reaction mixture is filtered, concentrated, and dissolved in heptane (20 0 ml). The heptane solution is passed through a short column of silica gel with heptane. Subsequent evaporation affords an oil which is crystallized from ethanol to yield 41.2 g (69%) of a white powder, m.p. 122°-6° C.

1. dry with materialThe organic phase is dried over magnesium sulfate
2. filtrationfiltered
3. temperaturethe mixture is refluxed for one hour
4. customWater is collected in a Dean-Stark trap
5. customThe entire reaction mixture
6. temperatureheating
7. filtrationThe colorless reaction mixture is filtered
8. concentrationconcentrated
9. dissolutiondissolved in heptane (20 0 ml)
10. customSubsequent evaporation
11. customaffords an oil which
12. customis crystallized from ethanol