HRID456178
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
To a solution 1-(3-((6-fluoro-1-methyl-1H-indazol-5-yl)methyl)imidazo[1,2-b]pyridazin-6-yl)propan-1-ol (13 mg, 0.015 mmol) in DCM (3 mL), was added TEA (0.011 ml, 0.079 mmol) and Dess-Martin periodinane (40 mg, 0.094 mmol). After stirring at rt for 10 min, the reaction was quenched with Na2SO3(aq), extracted with DCM. The organic layer was separated, dried over Na2SO4 and concentrated in vacuo to give a residue, which was purified by silica gel column chromatography with gradient Hex:EA to give 1-(3-((6-fluoro-1-methyl-1H-indazol-5-yl)methyl)imidazo[1,2-b]pyridazin-6-yl)propan-1-one (4 mg, 74%). LCMS (method A): [MH]+=338, tR=5.08 min.
WORKUP
后处理
- customthe reaction was quenched with Na2SO3(aq)
- extractionextracted with DCM
- customThe organic layer was separated
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuo
- customto give a residue, which
- customwas purified by silica gel column chromatography with gradient Hex