関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethylene carbonate | HCID 7303 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Hydroxy-5-methoxybenzaldehyde | HCID 5314561 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-(2-Hydroxy-ethoxy)-5-methoxy-benzaldehyde | HCID 86662039 | — |
反応手順
To a solution of 3-hydroxy-5-methoxy-benzaldehyde (12.0 g, 78.9 mmol) in anhydrous DMF (50 mL) was added [1,3]dioxolan-2-one (13.9 g, 157.0 mmol) and potassium carbonate (21.6 g, 157.0 mmol). The reaction mixture was then heated to 110° C. for 16 hours, then cooled to room temperature. Solid potassium carbonate was filtered and washed with ethyl acetate. The organic phase was collected and solvent was removed. The residue was purified by column chromatography (silica gel 230-400 mesh; eluting with 7:1 dichloromethane and ethyl acetate) to give 3-(2-hydroxy-ethoxy)-5-methoxy-benzaldehyde as a brown liquid. Yield: 10.0 g (65%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09238640B2 |
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| 出典データセット | uspto-grants-2016_01 |
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| ORD ID | ord-80a9783768c2446a9699767f2800eda5 |
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| 出典メモ | uspto-grants-2016_01 |
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