HRID251810

反应详情

EQUATION

反应方程式

HRID 251810 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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 was stirred at reflux for 4 h then cooled. Excess of solvent was removed in vacuo to afford the crude product. 2-chloroacetyl chloride (2 mmol) was added to the mixture solution of the crude product in Toluene (15 ml) at room temperature and then the mixture was heated to reflux for 5 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-(chloromethyl)-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 5 h
  7. concentrationThe mixture was concentrated in vacuo
  8. customthe crude product was purified by column chromatography on silica gel