HRID393660

反应详情

EQUATION

反应方程式

HRID 393660 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Phosphorous oxychloride (6.0 ml) was added to a stirred mixture of 2-acetamido-5-hydroxy-1,8-naphthyridine (2.4 g, 11.8 mmol) and N,N-dimethylaniline (6.0 ml) in toluene (100 ml). The mixture was then heated at reflux for 1 hour. The mixture was allowed to cool, the tolulene was removed by evaporation and the residue was partitioned between methylene chloride and aqueous sodium hydrogen carbonate solution. The organic layer was separated, dried (MgSO4) and the solvent was removed by evaporation to give 2-acetamido-5-chloro-1,8-naphthyridine (470 mg, 18%) as a brown solid.

WORKUP

后处理

  1. temperatureThe mixture was then heated
  2. temperatureat reflux for 1 hour
  3. temperatureto cool
  4. customthe tolulene was removed by evaporation
  5. customthe residue was partitioned between methylene chloride and aqueous sodium hydrogen carbonate solution
  6. customThe organic layer was separated
  7. dry with materialdried (MgSO4)
  8. customthe solvent was removed by evaporation