関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 2-Amino-5-nitrobenzoic acid | HCID 12032 | — |
| 反応物 | 2-tert-Butylbenzoyl chloride | HCID 13767186 | — |
| 生成物 | 2-(4-Tert-butylbenzoylamino)-5-nitrobenzoic acid | HCID 10497475 | 80% |
反応手順
To a mixture of 5-nitroanthranilic acid (24.6 g, 135 mmol) and pyridine (14.2 mL, 175 mmol) in N,N-dimethylformamide (140 mL) cooled to 0° C. was added tert-butylbenzoyl chloride (31.6 mL, 162 mmol). After stirring for 1 h, the reaction mixture was heated at 75° C. for 4 h, cooled, and poured into an ice/water mixture. The resulting solid was filtered, washed with water and a 1:2 mixture of diethyl ether/hexanes, and dried in vacuo at 150° C. for 2 h to give 37.1 g (80%) of the title compound as a light brown solid; mp 245-9° C. MS-FD m/e 342 (p) Analysis for C18H18N2O5: Calc: C, 63.15; H, 5.30; N, 8.18; Found: C, 62.85; H, 5.05; N, 8.48.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06605626B2 |
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| 出典データセット | uspto-grants-2003_08 |
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| ORD ID | ord-fa28e41d3d124130856f4769c30f5c29 |
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| 出典メモ | uspto-grants-2003_08 |
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