Hydrochloric Acid → 6-Chloro-2-(2,4-dichlorobenzoyl)-pyridine
Reaktionsgleichung
[Al+3].[Cl-].[Cl-].[Cl-].[Cl:5][C:6]1[N:11]=[C:10]([C:12](Cl)=[O:13])[CH:9]=[CH:8][CH:7]=1.[Cl:15][C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([Cl:22])[CH:17]=1.Cl>>[Cl:5][C:6]1[N:11]=[C:10]([C:12](=[O:13])[C:19]2[CH:20]=[CH:21][C:16]([Cl:15])=[CH:17][C:18]=2[Cl:22])[CH:9]=[CH:8][CH:7]=1Komponenten
5
Versuchsvorschrift
40.9 g AlCl3 is added in portions to a mixture of 26.4 g 6-chloro-2-pyridinecarboxylic acid chloride and 112 g 1,3-dichlorobenzene. The mixture is slowly heated until 130°-40° C. After standing overnight, it is added to a mixture of diluted HCl and crushed ice, basified and extracted with ethyl ether. The ethereal extracts are washed with water, dried and solvent evaporated (water pump). The residual deep green oil is crystallised from ethanol:water in the presence of decolorizing carbon. Yield: 10 g title compound, m.p. 103°-4° C.; UV (ethanol): λmax. 281 nm; ε: 14,500; Cl 37.02 (37.12).
Aufarbeitung
- temperatureThe mixture is slowly heated until 130°-40° C
- customcrushed ice
- extractionextracted with ethyl ether
- washThe ethereal extracts are washed with water
- customdried
- customsolvent evaporated (water pump)
- customThe residual deep green oil is crystallised from ethanol
Quellen und Nachweise
- ORD-Eintrag
- ord-cb360c11173540ef8be07646478bab67
- Quelldatensatz
- uspto-grants-1988_04
- Patentnummer
- US04736037
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