HRID69219

反应详情

EQUATION

反应方程式

HRID 69219 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-{4-[3-(7-Fluoro-quinolin-6-ylmethyl)-imidazo[1,2-b]pyridazin-6-yl]-pyrazol-1-yl}-piperidine-1-carboxylic acid tert-butyl ester (Stage 180.1, 850 mg, 1.611 mmol) was stirred 1 h at rt in dioxane (15 mL) with HCl in dioxane (4 M, 4,03 mL). The RM was then basified with saturated NaHCO3 aqueous sol. and the dioxane was evaporated. The resulting aqueous sol. was extracted 3 times with DCM containing 10% EtOH. Combined organic layers were dried and evaporated and the residue was purified by flash chromatography (CombiFlash® Companion System®, with RediSep® silica gel column, DCM/MeOH with ammonia=100:0->90:10) to afford the title compound (tR 3.04 min (conditions 3), MH+=428).

WORKUP

后处理

  1. customthe dioxane was evaporated
  2. extractionThe resulting aqueous sol. was extracted 3 times with DCM containing 10% EtOH
  3. customCombined organic layers were dried
  4. customevaporated
  5. customthe residue was purified by flash chromatography (CombiFlash® Companion System®, with RediSep® silica gel column, DCM/MeOH with ammonia=100:0->90:10)