Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Diethylene Glycol | HCID 8117 | — |
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Edukt | 1-(2-Fluoro(1,1'-biphenyl)-4-yl)ethan-1-one | HCID 6451918 | — |
| Lösungsmittel | O-Xylene | HCID 7237 | — |
| Produkt | 4-Ethyl-2-fluoro-1,1'-biphenyl | HCID 1490326 | 68% |
Reaktionsschritte
4-Acetyl-2-fluorobiphenyl (150 gram), 99% hydrazine hydrate (150 ml), potassium hydroxide (105 gram), digol (900 ml) and xylene (150 ml) were heated at 125° C. for 16 hours with stirring, after which the xylene and excess hydrazine hydrate were distilled until the internal temperature reached 165° C. The mixture was heated under reflux for three hours, cooled to 40° and poured into 5 liters of water. The product was extracted with petroleum ether (bp 60°-80°, 2×2 liter), the extract washed with water, dried over anhydrous sodium sulphate and evaporated. 4-Ethyl-2-fluorobiphenyl (95 gram, 68% theory) formed a colourless oil bp 130°/0.8 mm. Other 4-Alkyl-2-fluorobiphenyls were prepared by reaction of 2-fluoro-4-biphenylyl magnesium bromides with n-alkyl bromides and were colourless oils with the following properties listed in Table 5.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04695131 |
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| Quelldatensatz | uspto-grants-1987_09 |
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| ORD ID | ord-36378cc353d045b3b81aa262e2376455 |
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| Quellennotiz | uspto-grants-1987_09 |
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