Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Chlorodifluoromethane | HCID 6372 | — |
| Edukt | Tetrahydrofuran | HCID 8028 | — |
| Edukt | 4-Iodophenol | HCID 10894 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 1-(Difluoromethoxy)-4-iodobenzene | HCID 2737008 | — |
Reaktionsschritte
100 g (0.455 mol) of 4-iodophenol and 54.6 g (1.365 mol) of sodium hydroxide are added to a mixture of 300 ml of THF and 30 ml of water. After stirring for about 1/2 hour, the mixture is evaporated in a rotary evaporator; this is repeated after the addition of 200 ml of toluene. The residue is taken up in 400 ml of THF. The mixture is cooled to 0° C., 47.1 g (0.545 mol) of chlorodifluoromethane are introduced, and the mixture is then stirred for 1 hour. It is then stirred at about +5° C. for 18 hours. The solution above the resulting slurry-like precipitate was decanted off. It was evaporated in a rotary evaporator, and the residue was chromatographed through a silica gel column, using petroleum ether as eluent.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US05389292 |
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| Quelldatensatz | uspto-grants-1995_02 |
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| ORD ID | ord-a749331d7eec4c6295277b8e570169b7 |
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| Quellennotiz | uspto-grants-1995_02 |
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