HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methyl iodide → 1,2,4-Trifluoro-5-(methylsulfonyl)benzene
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methyl iodide | HCID 6328 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 2,4,5-Trifluorobenzenesulfinic acid | HCID 57241375 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 1,2,4-Trifluoro-5-(methylsulfonyl)benzene | HCID 46739396 | 71,1% |
Reaktionsschritte
To a solution of 2,4,5-trifluorobenzenesulfinic acid (34 g, 173 mmol), in DMF (200 mL), was added iodomethane (21.6 mL, 347 mmol), and N-ethyl-N-isopropylpropan-2-amine (60.5 mL, 347 mmol). The reaction mixture was stirred overnight at ambient temperature. The reaction was concentrated and partitioned between water and ethyl acetate and extracted with CH2Cl2. The combined organic layers were concentrated and purified over silica gel (15-100% EtOAc in hexanes) to afford 1,2,4-trifluoro-5-(methylsulfonyl)benzene (25.8 g, 123 mmol, 71% yield) as yellow solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08754226B2 |
| Quelldatensatz | uspto-grants-2014_06 |
| ORD ID | ord-4d3484d721434e5da22963726d069d9d |
| Quellennotiz | uspto-grants-2014_06 |