HRID1244317

反应详情

EQUATION

反应方程式

HRID 1244317 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.5 g 2,3-Diamino-6-methyl pyridine (4.0 mmol) and 0.37 g glycolic acid were heated at 150° C. for 1 h. The residue was suspended in chloroform (7.0 ml) treated with 1.5 ml thionyl chloride (20 mmol)for 4 h at reflux. The mixture was evaporated and the residue triturated with methanol. After concentration the residue was stirred over night in ether and the suspension was then filtered. The residue on the filter was dried to yield 0.67 g 2-chloromethyl-5-methyl-3H-imidazo[4,5-b]pyridine hydrochloride as a dark brown solid; M.p.: 225–230° C., (dec.).

WORKUP

后处理

  1. temperatureat reflux
  2. customThe mixture was evaporated
  3. customthe residue triturated with methanol
  4. concentrationAfter concentration the residue
  5. filtrationthe suspension was then filtered
  6. customThe residue on the filter was dried