HRID69219
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customthe dioxane was evaporated
- extractionThe resulting aqueous sol. was extracted 3 times with DCM containing 10% EtOH
- customCombined organic layers were dried
- customevaporated
- customthe residue was purified by flash chromatography (CombiFlash® Companion System®, with RediSep® silica gel column, DCM/MeOH with ammonia=100:0->90:10)