Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Cyclodecanone | HCID 73918 | — |
| Edukt | 1-Vinyl-1-cyclodecanol | HCID 13414161 | — |
| Produkt | Cyclododecanone | HCID 13246 | 52,8% |
Reaktionsschritte
0.5 g (2.7 mmol) of 1-vinyl-1-cyclodecanol (cf. I.1.3, comprises also about 8-10% cyclodecanone), quartz reactor 25/400 mm, temperature 670° C.±10, vaporization at 95-100° C. (airbath temperature) in about 10 min. Nitrogen stream about 2-2.5 l/h, vacuum 5-6 mbar. 0.45 g (90% crude yield) of a pure white condensate were obtained which partially crystallized into small fine needles. According to GC and GC/MS analyses, the mixture comprises, as main component, about 70% cyclododecanone, as well as 6-8% cyclodecanone and 2-3% starting material. Chromatographic separation of the mixture over silica gel (hexane/TBME 97:3) gave 0.26 g of cyclododecanone (52% isolated yield), which has identical retention times and spectroscopic properties as the commercially available compound (Fluka).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US06951964B2 |
|---|
| Quelldatensatz | uspto-grants-2005_10 |
|---|
| ORD ID | ord-c89e9f6bfd4a49d3afcc9402ff527586 |
|---|
| Quellennotiz | uspto-grants-2005_10 |
|---|