HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
tert-Butyl hydroperoxide → 8-alpha-Methylbenzyloxy-7,7,9,9-tetramethyl-8-aza-1,4-dioxaspiro[4.5]decane
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | tert-Butyl hydroperoxide | HCID 6410 | — |
| Edukt | Ethylbenzene | HCID 7500 | — |
| Edukt | 7,7,9,9-Tetramethyl-1,4-dioxa-8-azaspiro[4.5]decane | HCID 567045 | — |
| Katalysator | Molybdenum trioxide | HCID 14802 | — |
| Produkt | 8-alpha-Methylbenzyloxy-7,7,9,9-tetramethyl-8-aza-1,4-dioxaspiro[4.5]decane | HCID 53698547 | — |
Reaktionsschritte
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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05204473 |
| Quelldatensatz | uspto-grants-1993_04 |
| ORD ID | ord-b02e3cd813ba42e39ccb4e834ddc75bf |
| Quellennotiz | uspto-grants-1993_04 |