反应详情

温度

87.5 °C

A mixture of 15.0 g (0.09 mol) of 1-oxyl-4-hydroxy-2,2,6,6-tetramethylpiperidine and 126.6 g (1.15 mol) of cyclooctene is heated under a nitrogen atmosphere at 87-88° C. for 40 hours. The reaction mixture is filtered to remove 1,4-dihydroxy-2,2,6,6-tetramethylpiperidine, and the filtrate is washed with 5% ascorbic acid (2×50 mL) and distilled water (2×50 mL). The organic phase is dried over anhydrous magnesium sulfate and the volatiles removed in vacuo. The residue is crystallized from heptane to give 4.40 g (36% yield) of the title compound as a white solid.

1. filtrationThe reaction mixture is filtered
2. customto remove 1,4-dihydroxy-2,2,6,6-tetramethylpiperidine
3. washthe filtrate is washed with 5% ascorbic acid (2×50 mL)
4. distillationdistilled water (2×50 mL)
5. dry with materialThe organic phase is dried over anhydrous magnesium sulfate
6. customthe volatiles removed in vacuo
7. customThe residue is crystallized from heptane