Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Bromine | HCID 24408 | — |
| Edukt | Sodium hypobromite | HCID 23673712 | — |
| Edukt | HCID 178418543 | HCID 178418543 | — |
| Lösungsmittel | Sodium Hydroxide | HCID 14798 | — |
| Produkt | HCID 178418525 | HCID 178418525 | — |
Reaktionsschritte
A solution of sodium hypobromide was made by adding Br2 (1.01 ml, 39.5 mmol, 1.1 eq) slowly over a period of 5 min to NaOH (5N, 40 ml) that was previously cooled to 0° C. in an ice bath. The solution was stirred for 10 min before adding 2-hydroxynicotinic acid (5.0 g, 35.9 mmol) and placed in a 50° C. oil bath and stirred. Concurrently, a second pot of sodium hypobromide solution was made by slowly adding Br2 (1.01 ml, 39.5 mmol, 1.1 eq) to a NaOH solution (5N, 40 ml) in an ice bath. The second pot of sodium hypobromide was added to the solution of 2-hydroxynicotinic acid after 24 h of heating then was stirred for an additional 24 h. The solution was cooled to RT, placed in an ice bath and acidified with concentrated HCl while stirring. The precipitate which formed was filtered, washed and dried to afford the desired compound as an off-white solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08642624B2 |
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| Quelldatensatz | uspto-grants-2014_02 |
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| ORD ID | ord-79764d535c0b47359d2d5159489f4e7e |
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| Quellennotiz | uspto-grants-2014_02 |
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