関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 3-Iodo-5-(methoxycarbonyl)benzoic acid | HCID 15840391 | — |
| 溶媒 | Thionyl Chloride | HCID 24386 | — |
| 生成物 | Methyl 3-carbamoyl-5-iodobenzoate | HCID 21942671 | 82% |
反応手順
A solution of 3-methoxycarbonyl-5-iodobenzoic acid (3 g, 10 mmol) in thionyl chloride (2 mL) was heated for 2 hours at 60° C. The reaction mixture was cooled and concentrated in vacuo. The intermediate acid chloride was then diluted with tetrahydrofuran (10 mL) and cooled to 0° C. The mixture was then treated with a solution of 2M ammonia (20 mL, 40 mmol, methanol) and the reaction stirred for 1 hour at 0° C. The mixture was then filtered and the solvent removed in vacuo. Recrystallization from methanol afforded 2.5 g (82%) of 3-methoxycarbonyl-5-iodobenzamide, as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06660753B2 |
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| 出典データセット | uspto-grants-2003_12 |
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| ORD ID | ord-f0fdfc7412e84dd3aeba69830bed7f53 |
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| 出典メモ | uspto-grants-2003_12 |
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