関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 4-(2-Fluoroethoxy)benzaldehyde | HCID 15058649 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-(2-Fluoroethoxy)benzoic acid | HCID 51357093 | 63% |
反応手順
To a stirred solution of 50% w/v KOH (1.3 ml) and 4-(2-fluoroethoxy)benzaldehyde (0.5 g, 2.98 mmol) in MeOH (6 ml) at 65° C. was added dropwise over 20 min aqueous hydrogen peroxide (30 wt. % in water, 2.45 ml). On completion of the addition the reaction mixture was heated at 65° C. for a further 10 min. On cooling to room temperature, the reaction mixture was acidified with 1 M HCl and extracted with Et2O (3×30 ml). The combined organic extracts were washed with brine (30 ml), dried (Na2SO4) and the solvent removed under reduced pressure to give a solid which was purified by flash chromatography (1:1 Hexane/EtOAc) to give the title compound (0.278 g, 63%) as a colourless solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08895313B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-db5125dd0639494b9ee21fc6a3c480e7 |
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| 出典メモ | uspto-grants-2014_11 |
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