HRID383308

反应详情

EQUATION

反应方程式

HRID 383308 的结构方程式

PROCEDURE

实验过程

To a solution of 50% aq. chloroacetaldehyde (1.1 eq, 291 mmol, 37 ml) in ethanol (700 ml) is added 3-amino-6-chloro-pyridine (1 eq, 264 mmol, 34 g) at room temperature. The reaction mixture is refluxed for 3 hours. The solvent is removed in vacuo and the crude product is dissolved in water (400 ml). The aqueous solution is treated with sodium bicarbonate to pH=8 and extracted with dcm (3×250 ml), the organic layer is dried (MgSO4) and evaporated to give a brown solid (39.2 g) 6-chloro-imidazo[1,2-a]pyridine; [M+H]+153(155)

WORKUP

后处理

  1. temperatureThe reaction mixture is refluxed for 3 hours
  2. customThe solvent is removed in vacuo
  3. dissolutionthe crude product is dissolved in water (400 ml)
  4. additionThe aqueous solution is treated with sodium bicarbonate to pH=8
  5. extractionextracted with dcm (3×250 ml)
  6. dry with materialthe organic layer is dried (MgSO4)
  7. customevaporated