HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Chlorodifluoromethane → 4-(Difluoromethoxy)-2-fluoro-1-nitrobenzene
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Chlorodifluoromethane | HCID 6372 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 3-Fluoro-4-nitrophenol | HCID 520948 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 4-(Difluoromethoxy)-2-fluoro-1-nitrobenzene | HCID 46311593 | — |
Reaktionsbedingungen
| Temperatur | 85 °C |
|---|
Reaktionsschritte
N,N-Dimethylformamide (15 mL) was added to 3-fluoro-4-nitrophenol (1.01 g, 6.43 mmol) and potassium carbonate (5.33 g, 38.6 mmol) in a 50 mL stainless steel reactor. The vessel was sparged briefly with CF2HCl, chilled with dry ice, and then chlorodifluoromethane (3.34 g, 38.6 mmol) was transferred into the reactor through a polypropylene tube. The mixture was stirred at 85° C. for 2 hours. The supernatant mixture was concentrated onto silica gel. Purification via flash chromatography (0-40% ethyl acetate/hexanes) afforded the title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 8.28 (t, J=9.16 Hz, 1H), 7.51-7.57 (m, 1H), 7.50 (t, J=72.39 Hz, 1H), 7.21-7.29 (m, 1H)
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08546377B2 |
| Quelldatensatz | uspto-grants-2013_10 |
| ORD ID | ord-893f516ab94d49b893052899ed906033 |
| Quellennotiz | uspto-grants-2013_10 |