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 trioxide (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 (200 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 (200 ml)
10. customSubsequent evaporation
11. customaffords an oil which
12. customis crystallized from ethanol