HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Iodide → 2-Chloro-6-iodobenzoic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Iodide | HCID 4875 | — |
| Edukt | 2-Amino-6-chlorobenzoic acid | HCID 75071 | — |
| Edukt | Sodium Nitrite | HCID 23668193 | — |
| Lösungsmittel | Hydrochloric Acid | HCID 313 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Sulfuric Acid | HCID 1118 | — |
| Produkt | 2-Chloro-6-iodobenzoic acid | HCID 13399374 | 61% |
Reaktionsschritte
To the cold solution of 2-amino-6-chlorobenzoic acid (2.0 g, 11.6 mmol) in conc. HCl (10 mL) was added aq. solution of sodium nitrite (0.8 g, 11.6 mmol) at 0° C. followed by addition of solution of potassium iodide (2.88 g, 17.4 mmol) in water and conc. sulphuric acid (1 mL). The reaction mixture was refluxed for 2 h. The reaction mass was washed with sodium metabisulphate solution and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulphate and concentrated to afford 2.0 g of desired product. 1H NMR (300 MHz, DMSO d6): δ 7.08 (t, J=7.8 Hz, 1H), 7.42 (d, J=8.4 Hz, 1H), 7.76 (d, J=7.8 Hz, 1H), 8.37 (br s, 1H); MS (m/z): 280.59 (M)−.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09439890B2 |
| Quelldatensatz | uspto-grants-2016_09 |
| ORD ID | ord-b5abc99f45fb486487570d22a7f9cc1b |
| Quellennotiz | uspto-grants-2016_09 |