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3-Hydroxybenzaldehyde → 2-(3-Formyl-phenoxy)-4-methyl-benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Hydroxybenzaldehyde | HCID 101 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 2-Nitro-4-toluonitrile | HCID 96235 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(3-Formyl-phenoxy)-4-methyl-benzonitrile | HCID 21930410 | 36% |
反応手順
4-Methyl-2-nitrobenzonitrile (0.50 g, 3.1 mmol), 3-hydroxybenzaldehyde (0.38 g, 3.1 mmol) and cesium carbonate (1.00 g, 3.1 mmol) were heated with stirring in dry DMF (5 mL) at 80° C. for 28 h. The reaction mixture was cooled, poured into water and extracted with ethyl acetate. The ethyl acetate layer was separated, washed with 0.1N sodium hydroxide solution (3×), water (1×), brine (1×), and dried over MgSO4. After filtration, the solvent was removed in vacuo to yield 2-(3-formyl-phenoxy)-4-methyl-benzonitrile (0.26 g, 36%) as a brown resin, and was carried forward without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07119122B2 |
| 出典データセット | uspto-grants-2006_10 |
| ORD ID | ord-2376f183c6134766b7bf9e0bdc354ed6 |
| 出典メモ | uspto-grants-2006_10 |