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Water → 2-Phenylsulphenyl-4-trifluoromethylbenzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Thiophenol | HCID 7969 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Nitro-4-(trifluoromethyl)benzonitrile | HCID 69902 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Phenylsulphenyl-4-trifluoromethylbenzonitrile | HCID 18977984 | 85.2% |
反応手順
A mixture of 2-nitro-4-trifluoromethylbenzonitrile (8.64 g), thiophenol (4.4 g) and potassium carbonate (6.9 g) in acetonitrile was stirred at room temperature for 1 hour then heated at reflux for 9 hours. Thiophenol (0.3 ml) was added and the mixture was stirred and heated at reflux for 1 hour. Water was added and the mixture was extracted with dichloromethane, dried (MgSO4) and filtered. The flitrate was evaporated to dryness and the residue was recrystallized from n-hexane to give 2-(phenylsulphenyl)-4-trifluoromethylbenzonitrile (9.5 g) as a white solid, m.p. 51° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05424276 |
| 出典データセット | uspto-grants-1995_06 |
| ORD ID | ord-a692dcc491544bb0ae131d42e246b9a5 |
| 出典メモ | uspto-grants-1995_06 |