HRID649167

反应详情

EQUATION

反应方程式

HRID 649167 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 1-amino-5-chloroisoquinoline (10 g) in chloroform (150 ml) was added dropwise 3-chloro-2,4-pentanedione (11.3 g). The mixture was refluxed for 6 hours and then allowed to stand at room temperature over night. The mixture was washed successively with aqueous sodium bicarbonate and water, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by column chromatography on silica gel (200 g) with chloroform as an eluent to afford a solid. This solid was recrystallized from ethyl acetate to give 3-acetyl-7-chloro-2-methylimidazo[2,1-a]isoquinoline (1.3 g).

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 6 hours
  2. waitto stand at room temperature over night
  3. washThe mixture was washed successively with aqueous sodium bicarbonate and water
  4. dry with materialdried over magnesium sulfate
  5. customevaporated in vacuo
  6. customThe residue was purified by column chromatography on silica gel (200 g) with chloroform as an eluent
  7. customto afford a solid
  8. customThis solid was recrystallized from ethyl acetate