HRID887791
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
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-6-chloro-2-methyl-2H-indazole-4-carboxylate (330 mg, 1.09 mmol), palladium acetate (24.5 mg, 0.109 mmol), triphenylphosphine (57.2 mg, 0.218 mmol), potassium carbonate (226 g, 1.64 mmol) and methyl acrylate (147 μL, 1.64 mmol) in N,N-dimethylformamide (11 mL) was stirred with heating at 100° C. for 1 hr. The reaction solution 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=30/70→60/40) to give the title compound (270 mg, yield 80%).
WORKUP
后处理
- 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=30/70→60/40)