HRID5435

反应详情

EQUATION

反应方程式

HRID 5435 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixed solution of 10% potassium hydroxide (69.3 g, 105 mmoles) and dimethylsulfoxide (50 ml) was added S-[3-(amino)propyl]isothiourea.dihydrobromide (8.85 g, 39 mmoles) and the mixture was stirred at room temperature for 1.5 hours. To the reaction solution was added 5-chloroimidazo[1,2-a]pyridine (3.05 g, 20 mmoles), followed by stirring at room temperature for 1.5 hours and additional stirring at 65° C. for 20 hours. Water was added to the reaction solution, which was extracted with chloroform, washed several times with 1N-sodium chloride and dried over anhydrous magnesium sulfate. After the solvent was distilled off to obtain 2.66 g of the desired product (64.3%, pale yellow oily product).

WORKUP

后处理

  1. stirringby stirring at room temperature for 1.5 hours
  2. stirringadditional stirring at 65° C. for 20 hours
  3. extractionwas extracted with chloroform
  4. washwashed several times with 1N-sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationAfter the solvent was distilled off