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2,5-Dimethylthiophene → 2,5-Dimethylthiophene-3-carbaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,5-Dimethylthiophene | HCID 12514 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2,5-Dimethylthiophene-3-carbaldehyde | HCID 2762759 | — |
反応手順
To DMF (100 mL) stirred in an ice bath was added POCl3 (25 mL) drop wise followed by the addition of 2,5-dimethyl-thiophene (5 mL). The solution was warmed to room temperature and then was heated at 80° C. overnight. The reaction was cooled to room temperature and was slowly added to ice. Sodium acetate was added to bring the pH to between 5 and 6. The aqueous portion was extracted with ethyl acetate, and the organic portion was dried over sodium sulfate, concentrated under reduced pressure and purified on a silica gel column (eluent: 10:1:hexanes:EtOAc→4:1:hexanes:EtOAc to yield 2,5-dimethyl-thiophene-3-carboxaldehyde (1.5 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08563742B2 |
| 出典データセット | uspto-grants-2013_10 |
| ORD ID | ord-442415df1ea74f20aaaf2ca30bc9512b |
| 出典メモ | uspto-grants-2013_10 |