HRID1892371
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 of the 6-(1-ethoxyvinyl)-3-(1-(6-fluoro-1-methyl-1H-indazol-5-yl)ethyl)-imidazo[1,2-b]pyridazine (450 mg, 0.985 mmol) in acetic acid (8 mL) was added 3N HCl (0.5 mL). The solution was stirred at rt for 2 h and the solvent was removed under reduced pressure. The residue was diluted with water and its pH was adjusted to basic with aqueous NaHCO3 solution and extracted with DCM. The organic layer was washed with NaHCO3 (aq) and brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by column chromatography to give 300 mg (81%) of the title compound as a yellow solid. LCMS (method B): [MH]+=338, tR=2.49 min.
WORKUP
后处理
- customthe solvent was removed under reduced pressure
- additionThe residue was diluted with water and its pH
- extractionextracted with DCM
- washThe organic layer was washed with NaHCO3 (aq) and brine
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuo
- customThe residue was purified by column chromatography