Phosphorus oxychloride → HCID 20078039, 화합물

HRID 1654477노트

반응식

HRID 1654477 반응식
[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

참가 물질

3

반응물 2

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

생성물 1

HCID 20078039HCID 20078039, 화합물수율 82.9%

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-2aa9fdf89d114905b17ed5064d0acca4
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05407936

반응 노트

불러오는 중…