Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Sodium Iodide | HCID 5238 | — |
| Edukt | 4-Hydroxybiphenyl | HCID 7103 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | sodium thiosulfite anhydrous | HCID 15847209 | — |
| Edukt | Sodium Hypochlorite | HCID 23665760 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 4-Hydroxy-3-iodobiphenyl | HCID 4106140 | — |
Reaktionsschritte
Biphenyl-4-ol((5.26 g, 30.9 mmol), sodium iodide (4.635 g, 30.9 mmol), sodium hydroxide (1.276 g, 31.9 mmol) was dissolved in methanol (85 mL) and cooled to 0° C. To the solution was added 12% (w/v) sodium hypochlorite (20 mL) dropwise maintaining the temperature below 4° C. The solution was stirred at this temperature for 1 hour and then 2M sodium thiosulfite (50 mL) wad added and the pH of the solution was adjusted to >pH 7 with 1M HCl. The mixture was filtered and the filtrate was washed with water. The solid was dried in a vacuum oven and then the title product was obtained as crystals after recrystallisation from heptane. Yield 7.08 g, 77%.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07612068B2 |
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| Quelldatensatz | uspto-grants-2009_11 |
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| ORD ID | ord-015dc7f31fe34963ae9cf14d583f1eee |
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| Quellennotiz | uspto-grants-2009_11 |
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