HRID1978351

反应详情

EQUATION

反应方程式

HRID 1978351 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of ethyl (imidazo[1,2-a]pyridin-5-ylthio)acetate (11.8 g) in acetic acid (120 ml) was added hexamethylenetetramine (14.0 g) and the mixture was reacted at 90° C. for 10 hours. After this reaction mixture was allowed to cool, ethyl acetate (360 ml) was added and the mixture was washed with water. The organic layer was neutralized with 30% aqueous solution of sodium hydroxide under ice-cooling and washed again with water. The organic layer was concentrated and n-hexane (100 ml) was added to the crystalline residue, followed by 1 hour of stirring at room temperature. The crystals were collected by filtration and dried to provide the title compound (9.6 g, 78%).

WORKUP

后处理

  1. customthe mixture was reacted at 90° C. for 10 hours
  2. temperatureto cool
  3. washthe mixture was washed with water
  4. temperaturecooling
  5. washwashed again with water
  6. concentrationThe organic layer was concentrated
  7. additionn-hexane (100 ml) was added to the crystalline residue
  8. filtrationThe crystals were collected by filtration
  9. customdried