Phosphorus oxychloride → 5-Methylbenzimidazolone

HRID 1097127

반응식

HRID 1097127 반응식
[O:1]=[C:2]1[NH:6][C:5]2[CH:7]=[C:8]([C:11](OC)=O)[CH:9]=[CH:10][C:4]=2[NH:3]1.P(Cl)(Cl)(Cl)=O>O>[CH3:11][C:8]1[CH:9]=[CH:10][C:4]2[NH:3][C:2](=[O:1])[NH:6][C:5]=2[CH:7]=1

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 10352553methyl 2-oxo-2,3-dihydro-1H-1,3-benzodiazole-5-carboxylate

생성물 1

HCID 2231345-Methylbenzimidazolone

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Methyl 2-oxo-2,3-dihydro-1H-benzimidazole-6-carboxylate (43 g, 0.22 mol) was charged into phosphorus oxychloride (286 ml). Dry hydrogen chloride was bubbled through the boiling reaction mass for 12 hours. After cooling reaction mass was poured in mixture of ice and water (2 kg). Precipitate was filtered out. Filtrate was diluted with water (1.25 litres) and ammonia solution (˜800 ml). After that pH was adjusted to 5.6 with ammonia solution. Precipitate was filtered and rinsed with water. Yield 39.5 g (84%).

후처리

  1. customDry hydrogen chloride was bubbled through the boiling reaction mass for 12 hours
  2. temperatureAfter cooling
  3. customreaction mass
  4. filtrationPrecipitate was filtered out
  5. additionFiltrate was diluted with water (1.25 litres) and ammonia solution (˜800 ml)
  6. filtrationPrecipitate was filtered
  7. washrinsed with water

출처 및 근거

ORD 기록
ord-32acb0734e564e3ab0a4e2867ae69876
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08142863B2

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