Reaktionsgleichung
[Cl:1][C:2]1[C:10]([Cl:11])=[C:9]([O:12][C:13]([F:16])([F:15])[F:14])[CH:8]=[CH:7][C:3]=1[C:4](F)=[O:5].[OH2:17]>>[Cl:1][C:2]1[C:10]([Cl:11])=[C:9]([O:12][C:13]([F:16])([F:15])[F:14])[CH:8]=[CH:7][C:3]=1[C:4]([OH:17])=[O:5]Komponenten
3
Versuchsvorschrift
A suspension of crude 2,3-dichloro-4-trifluoromethoxybenzoyl fluoride (2 g, containing mixed antimony halides) in water was stirred vigorously for 24 hours. The mixture was extracted with dichloromethane and filtered. The organic layer was washed with hydrochloric acid (2M), aqueous sodium chloride solution and extracted into sodium carbonate solution (2M). The aqueous extract was acidified to pH 1 and the solid was filtered off and washed with water to give 2,3-dichloro-4-trifluoromethoxybenzoic acid (0.6 g) as a white solid mp 123°-126° C.
Aufarbeitung
- extractionThe mixture was extracted with dichloromethane
- filtrationfiltered
- washThe organic layer was washed with hydrochloric acid (2M), aqueous sodium chloride solution
- extractionextracted into sodium carbonate solution (2M)
- extractionThe aqueous extract
- filtrationthe solid was filtered off
- washwashed with water
Quellen und Nachweise
- ORD-Eintrag
- ord-20f8929b3f054551a66837e507bfa763
- Quelldatensatz
- uspto-grants-1998_05
- Patentnummer
- US05747424
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