反应详情

A mixture of 38.1 g (191 mmol) of 7,7,9,9-tetramethyl-8-aza-1,4-dioxaspiro[4.5]decane, 73.8 g (574 mmol) of 70% aq. t-butyl hydroperoxide, 2.0 g of molybdenum trioxide, and 130 ml of ethylbenzene is refluxed for 6 hours. Water is collected in a Dean-Stark trap. The catalyst is filtered and the filtrate is concentrated at reduced pressure. The residue is dissolved in heptane and passed through silica gel. A Kugelrohr distillation (120° C., 0.1 mm Hg) is used to remove volatile by-products. The title compound crystallizes on standing.

1. temperatureis refluxed for 6 hours
2. customWater is collected in a Dean-Stark trap
3. filtrationThe catalyst is filtered
4. concentrationthe filtrate is concentrated at reduced pressure
5. dissolutionThe residue is dissolved in heptane
6. distillationA Kugelrohr distillation (120° C., 0.1 mm Hg)
7. customto remove volatile by-products
8. customThe title compound crystallizes on standing