HRID1369560

反应详情

EQUATION

反应方程式

HRID 1369560 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
82.5 °C

PROCEDURE

实验过程

2,3-dimethyl-8-(2,6-dimethylbenzylamino)-imidazo[1,2-a]pyridine (2.0 g, 7.16 mmol) was dissolved in acetic acid (30 ml) and nitric acid (0.53 g, 7.57 mmol) was added. The mixture was heated to 80-85° C. and stirred for 3 h at this temperature. After evaporation of the major part of the acetic acid, the residue was partitioned between methylene chloride and water. The organic layer was washed with a solution of sodium carbonate and the solvent was removed under reduced pressure. The residue was dissolved in methylene chloride (100 ml) and filtered through silica gel (10 g) whereupon the methylene chloride was removed under reduced pressure. Chromatography with methylene chloride (100%) gave 0.4 g (17%) of the title compound.

WORKUP

后处理

  1. customAfter evaporation of the major part of the acetic acid
  2. customthe residue was partitioned between methylene chloride and water
  3. washThe organic layer was washed with a solution of sodium carbonate
  4. customthe solvent was removed under reduced pressure
  5. dissolutionThe residue was dissolved in methylene chloride (100 ml)
  6. filtrationfiltered through silica gel (10 g) whereupon the methylene chloride
  7. customwas removed under reduced pressure