Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Formic Acid | HCID 284 | — |
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | 3,4-Diaminobenzoic acid | HCID 69263 | — |
| Produkt | 5-Benzimidazolecarboxylic acid | HCID 459456 | — |
Reaktionsschritte
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%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08895118B2 |
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| Quelldatensatz | uspto-grants-2014_11 |
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| ORD ID | ord-44458fcf1f6a455f97193843b5ec03b8 |
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| Quellennotiz | uspto-grants-2014_11 |
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