HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methyl iodide → 5-Fluoro-2-nitroanisole
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methyl iodide | HCID 6328 | — |
| Edukt | 5-Fluoro-2-nitrophenol | HCID 9937 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 5-Fluoro-2-nitroanisole | HCID 2779250 | 82,7% |
Reaktionsschritte
To a solution of 4-fluoro-2-hydroxy-1-nitrobenzene (5.0 g, 31.8 mmol) in DMF (10 mL) was added K2CO3 (13.1 g, 95.4 mmol). The reaction mixture was stirred at RT for 1 h followed by addition of methyl iodide (9.93 g, 69.9 mmol) and the reaction mixture was stirred at 60° C. for 2 h. The reaction mass was concentrated and quenched in water. The reaction mass was basified with saturated sodium bicarbonate solution and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulphate and concentrated to afford 4.5 g of desired product. 1H NMR (300 MHz, DMSO d6): δ 3.93 (s, 3H), 6.97 (t, J=7.8 Hz, 1H), 7.31 (d, J=8.7 Hz, 1H), 8.02 (s, 1H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09439890B2 |
| Quelldatensatz | uspto-grants-2016_09 |
| ORD ID | ord-e8f86d536e734cf39f9dfc110116cfd1 |
| Quellennotiz | uspto-grants-2016_09 |