Hydrochloric Acid → 6-Chloro-2-(2,4-dichlorobenzoyl)-pyridine

HRID 648713Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 648713
[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]=1

Komponenten

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

  1. temperatureThe mixture is slowly heated until 130°-40° C
  2. customcrushed ice
  3. extractionextracted with ethyl ether
  4. washThe ethereal extracts are washed with water
  5. customdried
  6. customsolvent evaporated (water pump)
  7. 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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