HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 1-Chloro-2-fluoro-4-methoxy-5-nitrobenzene
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Methyl iodide | HCID 6328 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 4-Chloro-5-fluoro-2-nitrophenol | HCID 22503742 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 1-Chloro-2-fluoro-4-methoxy-5-nitrobenzene | HCID 53403289 | — |
Reaktionsschritte
4-Chloro-5-fluoro-2-nitrophenol (2.29 g, 12.0 mmol) was dissolved in DMF (25 mL). K2CO3 (2.5 g, 18 mmol) and iodomethane (0.893 mL, 14.3 mmol) were added and the mixture was stirred at rt overnight. The mixture was then poured into H2O and extracted with EtOAc (2×) and then the combined organics were extracted with H2O (5×). The organic layer was dried with MgSO4, filtered, and concentrated in vacuo to give the title compound of step B without further purification (2.19 g, 89%). 1H NMR (400 MHz, DMSO-d6) δ ppm 8.22 (dd, J=7.8, 1.0 Hz, 1H), 7.54 (d, J=11.4 Hz, 1H), 3.90 (d, J=1.1 Hz, 3H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08093239B2 |
| Quelldatensatz | uspto-grants-2012_01 |
| ORD ID | ord-53e6aceaee554e018d6d67e9b12ffe56 |
| Quellennotiz | uspto-grants-2012_01 |