HRID1097127

反应详情

EQUATION

反应方程式

HRID 1097127 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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%).

WORKUP

后处理

  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