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-2,3-dimethyl-2H-indazole-4-carboxylate (1.10 g, 3.89 mmol), palladium acetate (87.3 mg, 0.389 mmol), triphenylphosphine (204 mg, 0.778 mmol), potassium carbonate (591 mg, 4.28 mmol) and methyl acrylate (523 μL, 5.83 mmol) in N,N-dimethylformamide (39 mL) was stirred with heating at 100° C. for 4 hr. The solvent was evaporated under reduced pressure, and the residue was diluted with ethyl acetate, washed with water and saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/hexane=20/80→60/40) to give the title compound (606 mg, yield 54%).
WORKUP
后处理
- customThe solvent was evaporated under reduced pressure
- additionthe residue was diluted with ethyl acetate
- washwashed with water and saturated brine
- dry with materialdried over anhydrous sodium sulfate
- customThe solvent was evaporated under reduced pressure
- customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane=20/80→60/40)