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Water → 3-Methoxy-4-nitrobenzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Trifluoroacetic anhydride | HCID 9845 | — |
| 反応物 | 3-Methoxy-4-nitrobenzamide | HCID 11063338 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 3-Methoxy-4-nitrobenzonitrile | HCID 10899227 | — |
反応手順
To a solution of 3-methoxy-4-nitrobenzamide (8 g, 41 mmol) in dioxane (300 mL) was added pyridine (32 g, 408 mmol), followed by dropwise addition of trifluoroacetic anhydride (43 g, 204 mmol). The reaction mixture was stirred at room temperature for 5 h. Water was added to quench the reaction. The mixture was concentrated, then the residue was partitioned between ethyl acetate and water. The organic layer was separated, the aqueous layer was extracted with ethyl acetate. The organic layers were combined, washed with water, aqueous saturated CuSO4 solution, brine, dried over MgSO4, and concentrated to give 3-methoxy-4-nitrobenzonitrile as a off white solid (6.5 g, 90%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08217044B2 |
| 出典データセット | uspto-grants-2012_07 |
| ORD ID | ord-1ce235f726f643b6840bf88b14ef2b93 |
| 出典メモ | uspto-grants-2012_07 |