Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | 2-Amino-5-chloropyridine | HCID 66174 | — |
| Edukt | N-Iodosuccinimide | HCID 120273 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Lösungsmittel | Acetic Acid | HCID 176 | — |
| Produkt | 2-Amino-5-chloro-3-iodopyridine | HCID 11076010 | 97% |
Reaktionsschritte
A mixture of 6.43 g of 5-chloropyridin-2-ylamine and 12.38 g of N-iodosuccinimide in 300 ml of glacial acetic acid is heated at around 55° C. for 6 hours. After returning to a temperature of approximately 20° C., the mixture is agitated for approximately 18 hours and then concentrated to dryness under reduced pressure (13 kPa). The residue is taken up with 400 ml of water; the pH of the suspension obtained is brought back to approximately 8 by adding a saturated aqueous sodium hydrogen carbonate solution. The precipitate is filter-dried, washed with water, and dried at 40° C. under reduced pressure (13 kPa) for approximately 3 hours. 12.35 g of 5-chloro-3-iodopyridin-2-ylamine are obtained in the form of a solid, the characteristics of which are as follows:
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07528147B2 |
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| Quelldatensatz | uspto-grants-2009_05 |
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| ORD ID | ord-506e8cb1709847888265fbbfa270d949 |
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| Quellennotiz | uspto-grants-2009_05 |
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