HRID1639769
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 methyl 5-bromo-1H-indazole-4-carboxylate (2.00 g, 7.84 mmol) in ethyl acetate (80 mL) was added triethyloxonium hexafluorophosphate (2.92 g, 11.8 mmol), and the mixture was stirred under nitrogen atmosphere at room temperature for 15 hr. The reaction solution was diluted with ethyl acetate, saturated aqueous sodium hydrogen carbonate solution was added, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane=5/95→50/50) to give the title compound (2.03 g, yield 91%).
WORKUP
后处理
- additionwas added
- extractionthe mixture was extracted with ethyl acetate
- dry with materialThe extract was dried over anhydrous sodium sulfate
- customthe solvent was evaporated under reduced pressure
- customThe residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane=5/95→50/50)