HRID251807

反应详情

EQUATION

反应方程式

HRID 251807 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 0.5 mmol 3-(imidazo[1,2-b]pyridazin-2-yl)benzonitrile, 1 mmol NH2OH.HCl and 1 mmol Et3N in EtOH were stirred at reflux for 4 h then cooled. Excess of solvent was removed in vacuo to afford the crude product. Acetic anhydride (2 mmol) was added to the mixture solution of the crude product, THF (15 ml), and DMAP (cat.) at room temperature and then the mixture was heated to reflux for 12 h. The mixture was concentrated in vacuo and the crude product was purified by column chromatography on silica gel to give the 2-(3-(5-methyl-1,2,4-oxadiazol-3-yl)phenyl)imidazo[1,2-b]pyridazine.

WORKUP

后处理

  1. temperatureat reflux for 4 h
  2. temperaturethen cooled
  3. customExcess of solvent was removed in vacuo
  4. customto afford the crude product
  5. temperaturethe mixture was heated
  6. temperatureto reflux for 12 h
  7. concentrationThe mixture was concentrated in vacuo
  8. customthe crude product was purified by column chromatography on silica gel