Reaktionsgleichung
[Cl:1][C:2]1[CH:17]=[C:16]([C:18]([F:21])([F:20])[F:19])[CH:15]=[CH:14][C:3]=1[O:4][C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][CH:13]=1)[C:8]([OH:10])=[O:9].[CH3:22]O>>[Cl:1][C:2]1[CH:17]=[C:16]([C:18]([F:20])([F:19])[F:21])[CH:15]=[CH:14][C:3]=1[O:4][C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][CH:13]=1)[C:8]([O:10][CH3:22])=[O:9]Komponenten
3
Reaktionsbedingungen
- Temperatur
- 50 °C
Versuchsvorschrift
To a 300 ml, 3-necked flask equipped with a stirrer, gas bubbling tube, condenser, thermometer and drying tube is charged anhydrous methanol (100 ml) and 3-(2-chloro-4-trifluoromethylphenoxy)benzoic acid (12 g., 0.038 mole). Anhydrous hydrogen chloride gas is bubbled into the reaction mixture until the reaction temperature (exotherm) rises to 50° C. The reaction mixture is then maintained at 50° C. with external heating for 4 hours, then cooled, the solvent removed in vacuo and the residue dissolved in CCl4 (200 ml) and triturated with water (50 ml). The decanted and dried (anh. MgSO4) CCl4 layer is reduced in vacuo to give 12.2 g. of methyl 3-(2-chloro-4-trifluoromethylphenoxy)benzoate (98% yield).
Aufarbeitung
- customTo a 300 ml, 3-necked flask equipped with a stirrer
- customgas bubbling tube, condenser
- customthermometer and drying tube
- customAnhydrous hydrogen chloride gas is bubbled into the reaction mixture until the reaction temperature (exotherm)
- customrises to 50° C
- temperaturewith external heating for 4 hours
- temperaturecooled
- customthe solvent removed in vacuo
- dissolutionthe residue dissolved in CCl4 (200 ml)
- customtriturated with water (50 ml)
- customThe decanted
- dry with materialdried (anh. MgSO4) CCl4 layer
- customto give 12.2 g
Quellen und Nachweise
- ORD-Eintrag
- ord-934a86f90d964f338bc5f3d4af4a7a79
- Quelldatensatz
- uspto-grants-1977_06
- Patentnummer
- US04031131
Verknüpfte Notizen
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