Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Formic Acid | HCID 284 | — |
| Edukt | Hydrogen Peroxide | HCID 784 | — |
| Edukt | Cyclopentadiene | HCID 7612 | — |
| Edukt | 3,3,3-Trifluoro-2-(trifluoromethyl)-1-propene | HCID 91450 | — |
| Produkt | HCID 19097008 | HCID 19097008 | — |
Reaktionsschritte
5.2 g (20 mmol) of the Diels-Alder reaction product of 3,3,3-trifluoro-2-trifluoromethyl-1-propene (hexafluoroisobutene) and cyclopentadiene are mixed with 20 ml of formic acid, and 1.3 ml of 70 percent strength hydrogen peroxide (30 mmol) is added at 50° C., and the mixture is held at 50° C. for 20 hours. Testing for oxidant using KI-starch paper showed that the oxidant had been broken down completely. The low-boiling components are distilled off under reduced pressure. The residue is heated to 50° C. with 200 ml of 20% strength aqueous sodium hydroxide. The precipitated solid is extracted with a total of 130 ml of methylene chloride. The combined extracts are dried with magnesium sulfate, the methylene chloride is distilled off, and the residue is sublimated at 60° C. in an oil pump vacuum.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US05292971 |
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| Quelldatensatz | uspto-grants-1994_03 |
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| ORD ID | ord-af7162bf56cb43e9a873c7fd7f725eb5 |
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| Quellennotiz | uspto-grants-1994_03 |
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