Ethylene carbonate → HCID 20078042、化合物

HRID 1654480ノート

反応式

HRID 1654480 の反応式
[Cl:1][C:2]1[C:14]([N+:15]([O-:17])=[O:16])=[CH:13][C:5]2[N:6]([CH:10]([CH3:12])[CH3:11])[C:7](=O)[NH:8][C:4]=2[CH:3]=1.C1(=O)OCCO1.P(Cl)(Cl)([Cl:26])=O>>[Cl:26][C:7]1[N:6]([CH:10]([CH3:12])[CH3:11])[C:5]2[CH:13]=[C:14]([N+:15]([O-:17])=[O:16])[C:2]([Cl:1])=[CH:3][C:4]=2[N:8]=1

参加物

4

反応物 3

HCID 7303Ethylene carbonateHCID 24813Phosphorus oxychlorideHCID 19437878HCID 19437878、化合物

生成物 1

HCID 20078042HCID 20078042、化合物

実験手順

To 5-chloro-1-isopropyl-6-nitrobenzimidazol-2-one (1.0 g) were added ethylene carbonate (0.7 g) and phosphorus oxychloride (1.1 ml) and the mixture was refluxed for 5 hours. Phosphorus oxychloride was distilled off under reduced pressure and the residue was dissolved in ethyl acetate and the solution was added to ice-water and the mixture was neutralized with an aqueous sodium hydroxide solution. The organic layer was washed with water and dried over anhydrous magnesium sulfate and then the solvent was distilled off under reduced pressure to give 2,5-dichloro-1-isopropyl-6-nitrobenzimidazole (0.9 g). A part of the obtained product was recrystallized from ethanol, which showed the following physical properties:

後処理

  1. temperaturethe mixture was refluxed for 5 hours
  2. distillationPhosphorus oxychloride was distilled off under reduced pressure
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. additionthe solution was added to ice-water
  5. washThe organic layer was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-e59617c101cf49e9baea9c975557d953
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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