HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium percarbonate → 3,4-Difluorobenzoic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium percarbonate | HCID 159762 | — |
| Edukt | 3,4-Difluorobenzophenone | HCID 569908 | — |
| Lösungsmittel | Trifluoroacetic acid | HCID 6422 | — |
| Produkt | 3,4-Difluorobenzoic acid | HCID 99166 | 95,5% |
Reaktionsschritte
2.5 g of sodium percarbonate were added over 1 h to a solution of 2.2 g (10 mmol) of 3,4-difluorobenzophenone and 20 ml of trifluoroacetic acid (0° C.) and the temperature was then allowed to rise to 20° C. The mixture was stirred for 16 h at this temperature and 50 g of ice were then added. The mixture was subsequently extracted twice with dichloromethane and the organic phases were washed (NaHCO3) until the washings were neutral. The solvent was then removed. Working-up as described in Example 22 gave 1.2 g (7.6 mmol, 76%) of 3,4-difluorobenzoic acid, which can be obtained analytically pure from water (melting point 113°-120.5° C.).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05481032 |
| Quelldatensatz | uspto-grants-1996_01 |
| ORD ID | ord-3a540bda32044b3891e823049d0d41e1 |
| Quellennotiz | uspto-grants-1996_01 |