Phosphorus oxychloride → HCID 20078039、化合物

HRID 1654477ノート

反応式

HRID 1654477 の反応式
[Cl:1][C:2]1[CH:14]=[CH:13][C:5]2[N:6]([CH:10]([CH3:12])[CH3:11])[C:7](=O)[NH:8][C:4]=2[CH:3]=1.P(Cl)(Cl)([Cl:17])=O>>[Cl:17][C:7]1[N:6]([CH:10]([CH3:12])[CH3:11])[C:5]2[CH:13]=[CH:14][C:2]([Cl:1])=[CH:3][C:4]=2[N:8]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 108461602H-Benzimidazol-2-one, 5-chloro-1,3-dihydro-1-(1-methylethyl)-

生成物 1

HCID 20078039HCID 20078039、化合物収率 82.9%

実験手順

5-Chloro-1-isopropylbenzimidazol-2-one (81 g) in phosphorus oxychloride (207 g) was refluxed for 1 hour. The mixture was left to stand for cooling and then the reaction mixture was poured into ice-water and extracted with ethyl acetate. The ethyl acetate layer was washed with an aqueous sodium hydroxide solution, water and dried over anhydrous magnesium sulfate and then the solvent was distilled off under reduced pressure. To the residue was added acetonitrile (400 ml) and the insoluble material was removed by filtration and the solvent was distilled off under reduced pressure to give 2,5-dichloro-1-isopropylbenzimidazole (73 g). A part of the obtained product was subjected to silica gel column chromatography [eluted with chloroform] and recrystallized from hexane, which showed the following physical properties:

後処理

  1. waitThe mixture was left
  2. temperaturefor cooling
  3. extractionextracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with an aqueous sodium hydroxide solution, water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. additionTo the residue was added acetonitrile (400 ml)
  8. customthe insoluble material was removed by filtration
  9. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-2aa9fdf89d114905b17ed5064d0acca4
出典データセット
uspto-grants-1995_04
特許番号
US05407936

反応ノート

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