Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | Sodium chlorodifluoroacetate | HCID 2734985 | — |
| Edukt | 2-Bromo-5-hydroxypyridine | HCID 2762865 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Produkt | 2-Bromo-5-(difluoromethoxy)pyridine | HCID 23120579 | 43% |
Reaktionsschritte
Potassium carbonate (2.4 g, 17.3 mmols) and sodium chlorodifluoroacetate (4.2 g, 27.5 mmols) were added to a DMF (20 mL) solution of 2-bromo-5-hydroxypyridine (2.4 g, 13.8 mmols) and stirred overnight at 80° C. The reaction liquid was cooled to room temperature, added ether, washed with water and dried over anhydrous magnesium sulfate. Concentrating the solvent under reduced pressure, the resulting residue was purified on silica gel column chromatography (C-300; hexane:ethyl acetate=100:1-100:2) to provide the title compound (1.32 g, 43%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US07732456B2 |
|---|
| Quelldatensatz | uspto-grants-2010_06 |
|---|
| ORD ID | ord-a7269e992a824e05b5d1f6a6b677604a |
|---|
| Quellennotiz | uspto-grants-2010_06 |
|---|