HRID723402

反应详情

EQUATION

反应方程式

HRID 723402 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

34.8 ml of benzyl alcohol are added dropwise with ice cooling to a suspension of 13.5 g of sodium hydride (60% strength suspension in paraffin) in 510 ml of dimethylformamide and the mixture is stirred for 1 h until the evolution of gas is complete. 51.2 g of 6,8-dibromo-2,3-dimethylimidazo[1,2-a]pyridine are then introduced in small portions and the mixture is stirred at room temperature for 40 h. It is then poured onto 1 l of ice water, extracted three times with 100 ml of dichloromethane each time, the combined organic extracts are washed with saturated aqueous ammonium chloride solution and twice with water, concentrated to dryness in vacuo and the residue is stirred with a little ethyl acetate. The precipitate obtained here is filtered off and dried in vacuo. 43.2 g of the title compound of melting point 151–3° C. (ethyl acetate) are obtained.

WORKUP

后处理

  1. stirringthe mixture is stirred at room temperature for 40 h
  2. extractionextracted three times with 100 ml of dichloromethane each time
  3. washthe combined organic extracts are washed with saturated aqueous ammonium chloride solution and twice with water
  4. concentrationconcentrated to dryness in vacuo
  5. stirringthe residue is stirred with a little ethyl acetate
  6. customThe precipitate obtained here
  7. filtrationis filtered off
  8. customdried in vacuo