Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Methanol | HCID 887 | — |
| Edukt | 1,1,3,3,3-Pentafluoropropene | HCID 69647 | — |
| Katalysator | Di-tert-butyl peroxide | HCID 8033 | — |
| Produkt | 2,2,4,4,4-Pentafluorobutan-1-ol | HCID 10329622 | 77% |
Reaktionsschritte
Under nitrogen, into a quartz reactor equipped with a dry-ice condenser was added anhydrous methanol (100 g, 3.10 mol) and di-tertiarybutylperoxide (3.95 g, 0.015 mol). The quartz reactor tube was placed in a Rayonet UV photochemical reactor and HFC 1225, CF3CH═CF2 (57.9 g, 0.438 mol) was added drop-wise via a dry-ice condenser (−78° C.) over a period of ˜5 hours while being irradiated at 254 nm. After complete addition, the reaction mixture was irradiated for additional hour. Then the reaction mixture was concentrated under reduced pressure, the residue (˜65 g) was mixed well with 120 mL aq. Na2SO3 (20%), separated the lower layer, and washed with brine (40 mL). The crude product was then distilled under reduced pressure (24-28 mm Hg) to afford 55 g CF3CH2CF2CH2OH (yield 77% based on HFC 1225).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US06673976B1 |
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| Quelldatensatz | uspto-grants-2004_01 |
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| ORD ID | ord-2446fb5909434dbaa40d4f451f844b20 |
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| Quellennotiz | uspto-grants-2004_01 |
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