Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | 1-Dodecanol | HCID 8193 | — |
| Edukt | 1,4-Dioxane-2,6-dione | HCID 78232 | — |
| Lösungsmittel | Pyridine | HCID 1049 | — |
| Produkt | 1--Dodecyl hydrogen oxybisacetate | HCID 54089228 | — |
Reaktionsschritte
18.6 g n-dodecanol was dissolved in 25 ml pyridine on a steam bath. When 11.6 g of 1,4-dioxane-2,6-dione was added with stirring, the mixture quickly reached 80° C. After 5 minutes the solution was allowed to cool to room temperature and, after 2 hours, was poured into 200 ml 1 N HCl. The gel which precipitated was extracted with 300 ml ether, washed three times, with 0.1 N HCl and dried over Na2SO4. The ether was evaporated and the resulting clear oil was taken up in petroleum ether. Agitation and cooling under nitrogen precipitated a product which was separated by filtration. The remaining solution was diluted to 250 ml with petroleum ether for precipitation of a second crop. The yield totalled 18.1 g of a white crystalline solid that melted at 57°-59° C. and was soluble in acetone, chloroform, ether and/or methanol. Elemental analysis indicated 56.8% C; 8.5% H (Calc. 56.7% C; 8.5% H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04384969 |
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| Quelldatensatz | uspto-grants-1983_05 |
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| ORD ID | ord-cbb8bf3e570040b696ee7c9cceef77eb |
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| Quellennotiz | uspto-grants-1983_05 |
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