Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Acetic Anhydride | HCID 7918 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Hexahydrofuro(2,3-b)furan-3-ol | HCID 9898832 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | Hexahydrofuro[2,3-b]furan-3-yl acetate | HCID 21869022 | 90,7% |
Reaktionsschritte
Hexahydrofuro[2,3-b]furan-3-ol (IV, 60 g) was dissolved in dichloromethane (300 mL) and cooled to 0-5° C. To the cooled solution triethylamine (58.2 g), N,N-dimethylaminopyridine (1.12 g) was added, acetic anhydride (56.5 g) was added for 30-60 minutes at the same temperature, the mass temperature was raised to 25-35° C. and stirred for 2-4 hours. After completion of reaction the mass was cooled to 10-20° C., water (120 mL) was added, stirred for 30 minutes, separated the organic layer, washed with 10% sodium chloride solution (120 mL) and distilled out dichloromethane to get title compound (yield 72 g). Further, the product was purified by fractional distillation to get pure Hexahydrofuro[2,3-b]furan-3-yl acetate III (yield 54 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09216990B2 |
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| Quelldatensatz | uspto-grants-2015_12 |
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| ORD ID | ord-cca1ab0112f444b48d561ee32f866e66 |
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| Quellennotiz | uspto-grants-2015_12 |
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