Phosphorus oxychloride → 5-Methylbenzimidazolone

HRID 1097127

反応式

HRID 1097127 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 2231345-Methylbenzimidazolone

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-32acb0734e564e3ab0a4e2867ae69876
出典データセット
uspto-grants-2012_03
特許番号
US08142863B2

関連ノート

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