関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 5-Chloro-2-methylbenzoic acid | HCID 82009 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 5-chloro-2-methylbenzoate | HCID 20459600 | 96% |
反応手順
5-Chloro-2-methylbenzoic acid (46, 5.0 g, 29.3 mmol) was suspended in dichloromethane (30 mL) and thionyl chloride (3.2 mL, 5.2 g, 44 mmol) was added. The solution was stirred at room temperature for 1 hour. Methanol was added and the reaction was allowed to proceed for a further 16 hours. The volatile components were evaporated under reduced pressure. The resulting residue was taken up again in methanol (30 mL) and pyridine (5 mL) was added. The solution was stirred at room temperature for 2 days. The solvent was evaporated under reduced pressure. The residue was dissolved in dichloromethane and washed with water. The organic phase was dried over anhydrous magnesium sulfate, filtered, and concentrated to afford methyl 5-chloro-2-methylbenzoate (5.3 g, 96% yield) that was used in the following 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 | US07566718B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-538cf47b08b349e39490757c6154a296 |
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| 出典メモ | uspto-grants-2009_07 |
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