HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 2-Chloro-5-iodo-3-nitropyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Water | HCID 962 | — |
| Edukt | Ammonium Hydroxide | HCID 14923 | — |
| Edukt | 2-Amino-5-iodo-3-nitropyridine | HCID 3384468 | — |
| Edukt | Sodium Nitrite | HCID 23668193 | — |
| Katalysator | Cuprous chloride | HCID 62652 | — |
| Produkt | 2-Chloro-5-iodo-3-nitropyridine | HCID 1514294 | 43% |
Reaktionsschritte
To a solution of 5-iodo-3-nitropyridin-2-amine (1.3 g, 4.9 mmol) in concentrated HCl at 0° C. was added sodium nitrite (6.73 g, 97.13 mmol, 20 eq.) stepwise followed by the addition of copper(I) chloride (0.5 g, 4.9 mmol, 1 eq.) and the mixture was stirred at RT for 12 h. The mixture was then poured in to a mixture of ammonium hydroxide and water (1:1) and extracted with ethylacetate (3×150 ml). The combined organic layer was washed with water, aqueous sodium thiosulfate, brine and dried over sodium sulphate. The solvent was distilled off to afford the product in 43% yield (0.6 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09447091B2 |
| Quelldatensatz | uspto-grants-2016_09 |
| ORD ID | ord-fd868a0cfcec4c8d8f246e32aeb9792f |
| Quellennotiz | uspto-grants-2016_09 |