Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Formaldehyde | HCID 712 | — |
| Edukt | Cyclododecane | HCID 9268 | — |
| Edukt | Triphenylphosphine | HCID 11776 | — |
| Edukt | cis-1,5,9-Cyclododecatriene | HCID 86756482 | — |
| Lösungsmittel | Acetic Acid | HCID 176 | — |
| Produkt | Cyclododecene, (E)- | HCID 15164 | 97% |
Reaktionsschritte
A 70 ml autoclave equipped with a magnetic stirrer was charged with 40 g of trans-, trans-, cis-1,5,9-cyclododecatriene, 50 mg of RuCl3*H2O, 400 mg of triphenylphosphine, 0.5 g of 37% strength aqueous formaldehyde solution and 100 mg of acetic acid. The reactor was purged with nitrogen and hydrogen and then brought to a hydrogen pressure of 20 bar and heated up with stirring. At 115° C., the reactor pressure decreased noticeably and the internal temperature rose quickly to 140° C. Thereafter the reactor was constantly maintained at 20 bar and 145° C. by means of hydrogen. After about 2.5 hours the reactor was cooled down and decompressed. The effluent was found by GC to contain a yield of 97% of cyclododecene and 1.8% of cyclododecane. The remainder was cyclododecadiene.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US06194624B1 |
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| Quelldatensatz | uspto-grants-2001_02 |
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| ORD ID | ord-db63a81a123e443cb48b349494f99c26 |
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| Quellennotiz | uspto-grants-2001_02 |
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