Chloroform → 3-(4,5-dichloro-1H-imidazol-2-yl)pyridine

HRID 1439247ノート

反応式

HRID 1439247 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[NH:8]C=[CH:10][N:11]=2)[CH:2]=1.[Cl:12]N1C(=O)CCC1=O.[CH:20]([Cl:23])(Cl)Cl>>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[NH:8][C:20]([Cl:23])=[C:10]([Cl:12])[N:11]=2)[CH:2]=1

参加物

4

反応物 3

HCID 6212ChloroformHCID 31398ChlorosuccinimideHCID 123955003-(1H-Imidazol-2-yl)pyridine

生成物 1

HCID 213989023-(4,5-dichloro-1H-imidazol-2-yl)pyridine

実験手順

To a suspension of 2-(3-pyridyl)-imidazole (1.5 g., 0.01 moles) in chloroform (150 ml.) is added dropwise with stirring over one hour at reflux N-chlorosuccinimide (2.6 g., 0.02 moles). The reaction mixture is heated three hours at reflux. After cooling, the solvent is removed at 20 mm. and the residue triturated with water while heating on a steam bath. The resulting solid is filtered and after recrystallization from acetonitrile 400 mg. of 2-(3-pyridyl)-4,5-dichloroimidazole is obtained, m.p. 237°-238° C.

後処理

  1. additionis added dropwise
  2. temperatureThe reaction mixture is heated three hours
  3. temperatureat reflux
  4. temperatureAfter cooling
  5. customthe solvent is removed at 20 mm
  6. customand the residue triturated with water
  7. temperaturewhile heating on a steam bath
  8. filtrationThe resulting solid is filtered
  9. customafter recrystallization from acetonitrile 400 mg

出典と根拠

ORDレコード
ord-6b62ec7126eb43fb85506213ab94d354
出典データセット
uspto-grants-1977_11
特許番号
US04058614

反応ノート

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