HRID69297

反应详情

EQUATION

反应方程式

HRID 69297 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-[6-(1-Methyl-1H-pyrazol-4-yl)-imidazo[1,2-b]pyridazin-3-ylmethyl]-imidazo[1,2-a]pyridine-3-carbaldehyde (Example 297, 50 mg, 0.140 mmol) was dissolved in MeOH (3 mL) and water (1 mL) then NaBH4 (2.6 mg, 0.070 mmol) was added. The RM was stirred at rt for 30 min. It was quenched with water and EtOAc. The precipitate formed was filtered off. The filtrate was concentrated then was triturated with MeOH. The salt was filtered off. The filtrate was concentrated and then triturated again with Et2O, The precipitate was filtered off and it was purified by flash chromatography (CombiFlash® Companion System®, with RediSep® silica gel column, 0 to 20% MeOH in DCM) to afford after evaporation of the solvent the title compound as a yellow solid (tR 0.6 min (conditions 2), MH+=360).

WORKUP

后处理

  1. customIt was quenched with water and EtOAc
  2. customThe precipitate formed
  3. filtrationwas filtered off
  4. concentrationThe filtrate was concentrated
  5. customthen was triturated with MeOH
  6. filtrationThe salt was filtered off
  7. concentrationThe filtrate was concentrated
  8. customtriturated again with Et2O
  9. filtrationThe precipitate was filtered off
  10. customit was purified by flash chromatography (CombiFlash® Companion System®, with RediSep® silica gel column, 0 to 20% MeOH in DCM)
  11. customto afford
  12. customafter evaporation of the solvent the title compound as a yellow solid (tR 0.6 min (conditions 2), MH+=360)