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

HRID 65528

反応式

HRID 65528 の反応式
[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

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 109431,3-DichlorobenzeneHCID 6451240Aluminum(III) ChlorideHCID 109429766-chloropyridine-2-carbonyl Chloride

生成物 1

HCID 201457146-Chloro-2-(2,4-dichlorobenzoyl)-pyridine

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-1e606b91cf6d41398a9a4167ddca2ab4
出典データセット
uspto-grants-1986_09
特許番号
US04614833

関連ノート

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