HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Phosgene → 6-Fluoro-1,3-benzoxazol-2(3H)-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Phosgene | HCID 6371 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 2-Amino-5-fluorophenol | HCID 185763 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 6-Fluoro-1,3-benzoxazol-2(3H)-one | HCID 14457358 | 96% |
Reaktionsschritte
To 5.0 g (39.3 mmol) 2-amino-5-fluorophenol in 150 ml of CH2Cl2 at 0° C. was added 13.4 (98 mmol) of potassium carbonate and 23 g (47 mmol) of 20 wt. % phosgene in toluene. After warming to room temperature, the reaction was stirred an additional hour before quenching onto 200 ml ice/water. The layers were separated and the aqueous phase was extracted with EtOAc (1×100 ml) before the organics were combined and dried over Na2SO4. The solvent was removed in vacuo to give 5.76 g (96% yield) of the desired product as determined by 1H NMR.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05393735 |
| Quelldatensatz | uspto-grants-1995_02 |
| ORD ID | ord-c0d0f216f7a4464b823006ecd68e6c7a |
| Quellennotiz | uspto-grants-1995_02 |