関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 5-Chloro-2-methyl-3-nitrobenzoic acid | HCID 23009762 | — |
| 生成物 | Methyl 5-chloro-2-methyl-3-nitrobenzoate | HCID 53399191 | 90% |
反応手順
To a stirred solution of 5-chloro-2-methyl-3-nitrobenzoic acid (1 equiv.) in DMF (3 ml per 1 mmol), iodomethane (4 equiv.) and sodium carbonate (4 equiv.) were added. The resulting reaction mixture was stirred at 60° C. for 8 h. On completion, the reaction mixture was filtered and the inorganic solid residue washed with ethyl acetate. The combined filtrate was concentrated under vacuum till dryness. The residue was re-dissolved in ethyl acetate and washed with 5% sodium bicarbonate solution followed by 5M HCl solution. Organic layer was finally washed with brine, dried over sodium sulfate and concentrated to afford pure methyl 5-chloro-2-methyl-3-nitrobenzoate (90-95%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09206157B2 |
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| 出典データセット | uspto-grants-2015_12 |
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| ORD ID | ord-ac012fbd129241c5baccfa8f1a71d5b9 |
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| 出典メモ | uspto-grants-2015_12 |
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