HRID887742
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
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
A suspension of methyl 5-bromo-2-methyl-2H-indazole-4-carboxylate (1.65 g, 6.18 mmol), palladium acetate (139 mg, 0.62 mmol), triphenylphosphine (325 mg, 1.24 mmol), potassium carbonate (1.28 g, 9.27 mmol) and methyl acrylate (834 μL, 9.27 mmol) in N,N-dimethylformamide (60 mL) was stirred with heating at 100° C. for 50 min. The reaction solution was diluted with water, extracted with ethyl acetate, washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/hexane=30/70→70/30) to give the title compound (1.33 g, yield 78%).
WORKUP
后处理
- extractionextracted with ethyl acetate
- washwashed with water and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- customThe solvent was evaporated under reduced pressure
- customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane=30/70→70/30)