HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 2-[(3,5-Dimethylphenyl)sulfonyl]-6-fluorobenzenecarbonitrile
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | 2-[(3,5-Dimethylphenyl)thio]-6-fluorobenzonitrile | HCID 10848751 | — |
| Edukt | Potassium hydroxy sulfite | HCID 23707502 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 2-[(3,5-Dimethylphenyl)sulfonyl]-6-fluorobenzenecarbonitrile | HCID 486357 | 65% |
Reaktionsschritte
2-[(3,5-Dimethylphenyl)thio]-6-fluorobenzonitrile (Example 18) (1.0 g 3.9 mmol) was dissolved in 100 ml of methanol. A solution of OXONE®.dagger. (5.26 g, 8.6 mmol) in 30 ml of water was added dropwise with stirring. After stirring 1 h, another 1.5 equivalents of OXONE® (3.60 g 5.9 mmol) was added. The reaction was stirred for 18 h. The solid was removed by vacuum filtration and washed with 200 ml of methanol, then with 2×60 ml of acetone. The filtrate was concentrated to dryness and chromatographed on silica gel (flash; Hex/EtOAc 1:1) to provide 0.73 g (65%) of 2-[(3,5-dimethylphenyl)sulfonyl]-6-fluorobenzonitrile: mp 167°-168° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05723452 |
| Quelldatensatz | uspto-grants-1998_03 |
| ORD ID | ord-3a63765ce57f4be88697886cd8f75569 |
| Quellennotiz | uspto-grants-1998_03 |