関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,4-Dimethylbenzoic acid | HCID 11897 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 触媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | Methyl 2,4-dimethylbenzoate | HCID 32031 | — |
反応手順
2,4-dimethylbenzoic acid (20.0 g) was suspended in chloroform (100 ml), and thereto were added oxalyl chloride (6.8 ml) and N,N-dimethylformamide (2 drops). The mixture was stirred at room temperature overnight. The solvent was evaporated under reduced pressure, and the residue was dissolved in methanol (200 ml). The mixture was stirred at room temperature for 3 hours. The solvent was evaporated under reduced pressure, and the residue was dissolved in ethyl acetate. The mixture was washed successively with a saturated aqueous sodium hydrogen carbonate solution and brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure to give methyl 2,4-dimethylbenzoate as pale yellow oil, which was used in the subsequent step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08785403B2 |
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| 出典データセット | uspto-grants-2014_07 |
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| ORD ID | ord-b9fa98f2bcf44b5cabbfc1ecb919a6f0 |
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| 出典メモ | uspto-grants-2014_07 |
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