Reaktionsgleichung
[H-].[Na+].[Cl:3][C:4]1[CH:9]=[C:8]([O:10][C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([C:17]([F:20])([F:19])[F:18])[CH:12]=2)[CH:7]=[CH:6][C:5]=1[OH:21].Cl[C:23]1[CH:28]=[CH:27][C:26](CCl)=[CH:25][N:24]=1.[CH3:31]N(C)C=O>>[Cl:3][C:4]1[CH:9]=[C:8]([O:10][C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([C:17]([F:19])([F:20])[F:18])[CH:12]=2)[CH:7]=[CH:6][C:5]=1[O:21][CH2:31][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=1Komponenten
Versuchsvorschrift
To a solution 0.07 g of sodium hydride (60% oil dispersion) in 10 ml of N,N-dimethylformamide, there was added dropwise a solution of 0.50 g of 2-chloro-4-(3-trifluoromethylphenoxy)phenol in 3 ml of N,N-dimethylformamide with stirring and ice-cooling. After 30 minutes, a solution of 0.28 g of 2-chloro-5-chloromethylpyridine in 5 ml of N,N-dimethylformamide was added thereto at room temperature, followed by stirring at the same temperature for 10 hours. The reaction mixture was poured into ice-water and extracted twice with 100 ml of ethyl acetate. The extracts were combined together, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography to give 2-chloro-5[[2-chloro-4-(3-trifluoromethylphenoxy)phenoxy]methylpyridine.
Aufarbeitung
- temperatureice-cooling
- customat room temperature
- stirringby stirring at the same temperature for 10 hours
- extractionextracted twice with 100 ml of ethyl acetate
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-7408419a1219444fa4bd65ef2386ffca
- Quelldatensatz
- uspto-grants-1992_09
- Patentnummer
- US05151428
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