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Water → 5-Methoxy-2-(methylsulfanyl)benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Fluoro-5-methoxybenzonitrile | HCID 2774546 | — |
| 反応物 | Sodium methanethiolate | HCID 4378561 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-Methoxy-2-(methylsulfanyl)benzonitrile | HCID 66877736 | 70% |
反応手順
(Step 1) A mixture of 2-fluoro-5-methoxybenzonitrile (10 g) and sodium methanethiolate (5.1 g) was stirred in N,N-dimethylformamide (20 ml) at 60° C. for 3 hr. The reaction solution was treated with water, and extracted with ethyl acetate. The extract was washed successively with 1N hydrochloric acid, aqueous sodium hydrogen carbonate solution and saturated brine, and dried over magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was crystallized from ethyl acetate-hexane to give 5-methoxy-2-(methylsulfanyl)benzonitrile (8.3 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07982044B2 |
| 出典データセット | uspto-grants-2011_07 |
| ORD ID | ord-95a5a53467594f6a9ff36021ec546772 |
| 出典メモ | uspto-grants-2011_07 |