反应详情

温度

100 °C

A mixture of 29.4 g (0.17 mol) of 1-oxyl-4-hydroxy-2,2,6,6-tetramethylpiperidine and 148.0 g (1.37 mol) of 1,5-cyclooctadiene is heated under a nitrogen atmosphere at 100° C. for 24 hours. The reaction mixture is filtered to remove 1,4-dihydroxy-2,2,6,6-tetramethylpiperidine, and the filtrate is diluted with heptane (250 mL). The organic phase 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 chromatographed to give 8.1 g (33% 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. additionthe filtrate is diluted with heptane (250 mL)
4. washThe organic phase is washed with 5% ascorbic acid (2×50 mL)
5. distillationdistilled water (2×50 mL)
6. dry with materialThe organic phase is dried over anhydrous magnesium sulfate
7. customthe volatiles removed in vacuo
8. customThe residue is chromatographed