関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3,4-Diaminobenzoic acid | HCID 69263 | — |
| 生成物 | 5-Benzimidazolecarboxylic acid | HCID 459456 | — |
反応手順
3,4-Diaminobenzoic acid (20 g, 0.13 mol) was suspended in formic acid (120 ml) while cooling. After that hydrochloric acid (12 ml) was added. An obtained reaction mass was agitated for 24 hours at a room temperature. Reaction mixture was filtered through fiber glass filter. Then filter cake was dissolved in water (400 ml), pH was adjusted to 2.0 with ammonia solution and reaction mass was agitated overnight. Resulting suspension was filtered, pH of filtrate was adjusted to 3.0 with ammonia solution and reaction mass was agitated for two hours. Precipitate was filtered and dried at ˜100° C. H1NMR (Brucker Avance-300, DMSO-d6, δ, ppm): 7.695 (d, H, CHAr(7)); 7.877 (dd, H, CHAr(6)); 8.25 (d, H, CHAr(4)); 8.44 (s, H, (s, H, CHAr(2)); 12.82 (s, 2H, NH, COOH). Yield was 11.3 g (54%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08895118B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-44458fcf1f6a455f97193843b5ec03b8 |
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| 出典メモ | uspto-grants-2014_11 |
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