HRID69167

反应详情

EQUATION

反应方程式

HRID 69167 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl magnesium bromide (3 M in Et2O, 333 μL, 1 mmol) was added to a solution of 3-bromo-6-chloro-imidazo[1,2-b]pyridazine (116 mg, 0.5 mmol) in THF (5 mL) at rt . The RM was stirred for 30 min and imidazo[1,2-a]pyridine-6-carbaldehyde (154 mg, 2 mmol) in THF (3 mL) was added dropwise. After 1 h the RM was extracted with a solution of NH4Cl and EtOAc. The combined organic phases were dried over Na2SO4, concentrated under reduced pressure, and purified by flash chromatography (CombiFlash® Companion System®, with RediSep® silica gel column, Hexane/EtOAc=95:5->0:100) to afford the title compound as a yellowish crystalline compound (tR 2.72 min (conditions 3), MH+=300.2).

WORKUP

后处理

  1. extractionAfter 1 h the RM was extracted with a solution of NH4Cl and EtOAc
  2. dry with materialThe combined organic phases were dried over Na2SO4
  3. concentrationconcentrated under reduced pressure
  4. custompurified by flash chromatography (CombiFlash® Companion System®, with RediSep® silica gel column, Hexane/EtOAc=95:5->0:100)