関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Benzyl Bromide | HCID 7498 | — |
| 反応物 | o-Vanillin | HCID 8991 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 触媒 | Potassium Iodide | HCID 4875 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(Benzyloxy)-3-methoxybenzaldehyde | HCID 1268087 | 81% |
反応手順
Benzyl bromide (8.6 ml) was added to a stirred solution of 3-methoxysalicylaldehyde (10 g), potassium carbonate (14.76 g) and potassium iodide (0.12 g) in DMF (120 ml) under an atmosphere of argon. The reaction was heated at 70° C. for 16 hours. Water (200 ml) was added causing the precipitation of a brown oil which crystallised on cooling. The solid was filtered, washed with water, dissolved in dichloromethane and dried (MgSO4). The solvent was removed in vacuo to give an oil which crystallised on trituration with iso-hexane to give the product as an off white solid (12.85 g, 81%); NMR d (CD3SOCD3) 3.91 (s, 3H), 5.15 (s, 2H), 7.14-7.22 (m, 2H), 7.29-7.42 (m, 6H), 10.10 (t, 1H); M/z (+) 243 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06569888B1 |
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| 出典データセット | uspto-grants-2003_05 |
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| ORD ID | ord-85cf6ef0ec784178b2581fde72b3ab84 |
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| 出典メモ | uspto-grants-2003_05 |
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