関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Butanethiol | HCID 10560 | — |
| 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-(1-Methylpropylsulphenyl)-4-trifluoromethylbenzonitrile | HCID 54339387 | 74.9% |
反応手順
2-Nitro-4-trifluoromethylbenzonitrile (10.8 g) and potassium carbonate (8.3 g) were heated to reflux in acetonitrile. A solution of 1-methylpropanethiol (5 g) in acetonitrile was added. The resultant suspension was heated at reflux for 4.5 hours. After cooling water was added and the mixture extracted with ethyl acetate. The organic extracts were washed with water. The organic extracts were washed with water, dried (anhydrous magnesium sulphate) and filtered. The filtrate was evaporated to dryness and the residue purified by column chromatography eluting with ethyl acetate in cyclohexane to give 2-(1-methylpropylsulphenyl)-4-trifluoromethylbenzonitrile (9.7 g) as a yellow oil, NMR (CDCl3) 1.0(t,3H), 1.2(d,3H), 1.5(m,1H), 3.4(m,1H), 7.3(m,1H), 7.6(m,2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05859283 |
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| 出典データセット | uspto-grants-1999_01 |
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| ORD ID | ord-7313a217b7904498bbf2938ee746f5c3 |
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| 出典メモ | uspto-grants-1999_01 |
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