Phosphorus oxychloride → 2-Chloro-4-phenylthiazole
Reaktionsgleichung
O[C:2]1[S:3][CH:4]=[C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:6]=1.P(Cl)(Cl)([Cl:15])=O>>[Cl:15][C:2]1[S:3][CH:4]=[C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:6]=1Komponenten
3
Versuchsvorschrift
To 80 ml of phosphorus oxychloride were added 7.7 g (43 mmol) of 2-hydroxy-4-phenylthiazole, followed by heating at 100°-105° C. for 2 hours. The solvent was then distilled off from the reaction mixture under reduced pressure. Ice water was added to the residue, followed by extraction with ethyl ether. The ether layer was washed with water. After purification by silica gel column chromatography (solvent: hexane/ethyl acetate=5/1), the title compound was obtained as pale yellow crystals.
Aufarbeitung
- temperatureby heating at 100°-105° C. for 2 hours
- distillationThe solvent was then distilled off from the reaction mixture under reduced pressure
- additionIce water was added to the residue
- extractionfollowed by extraction with ethyl ether
- washThe ether layer was washed with water
- customAfter purification by silica gel column chromatography (solvent: hexane/ethyl acetate=5/1)
Quellen und Nachweise
- ORD-Eintrag
- ord-bbd48428ddad4311a4e64414339d0545
- Quelldatensatz
- uspto-grants-1992_05
- Patentnummer
- US05112841
Notizen zur Reaktion
Wird geladen…