参与物
| 角色 | 名称 | HCID | 投料 |
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| 反应物 | 甲酸 | HCID 284 | — |
| 反应物 | 海萝胶 | HCID 313 | — |
| 反应物 | 3,4-二氨基苯甲酸 | HCID 69263 | — |
| 产物 | 1H-苯并咪唑-5-羧酸 | HCID 459456 | — |
反应步骤
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%).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US08895118B2 |
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| 来源数据集 | uspto-grants-2014_11 |
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| ORD ID | ord-44458fcf1f6a455f97193843b5ec03b8 |
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| 来源说明 | uspto-grants-2014_11 |
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