Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Propionic Acid | HCID 1032 | — |
| Edukt | Vinyl Acetate | HCID 7904 | — |
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | 3,3-Bis(hydroxymethyl)oxetane | HCID 529229 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 3,3-Bis(vinyloxymethyl)oxetane | HCID 25158284 | 90% |
Reaktionsschritte
A mixture (280 ml) of 24.9 g (0.23 mol) of sodium carbonate with toluene was raised in temperature to 95° C., 1.4 g of propionic acid was added, and, while maintaining the temperature at 95° C., 16 g of vinyl acetate was added dropwise, and 15 minutes later, 1.27 g (1.9 mmol) of di-μ-chlorobis(1,5-cyclooctadiene)diiridium(I) [Ir(cod)Cl]2 was further added. Next, 40 g (0.19 mol) of oxetane-3,3-dimethanol was added dropwise over 3 hours for a reaction. After the completion of the dropwise addition and subsequent stirring for 1 hour, the reaction mixture was analyzed by gas chromatography and found that there were formed 3,3-bis(vinyloxymethyl)oxetane represented by the following formula in a yield of 90% and (3-vinyloxymethyloxetan-3-yl)methanol in a yield of 2%. The reaction mixture was purified by distillation and thereby yielded 31 g of 3,3-bis(vinyloxymethyl)oxetane with a purity of 99%.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08975349B2 |
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| Quelldatensatz | uspto-grants-2015_03 |
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| ORD ID | ord-7fe1e2759a4f451cadff055525ab1027 |
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| Quellennotiz | uspto-grants-2015_03 |
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