HRID1804827
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
- 70 °C
PROCEDURE
实验过程
Preparation 2: A solution of 2-(5-methyl-1H-pyrazol-3-yl)pyridine (500 mg, 3.15 mmol) in acetonitrile (912 mL) was treated with N-chlorosuccinimide in 6 portions and the resulting mixture stirred at 70° C. for 14 h. The mixture was cooled and then concentrated in vacuo to yield a residue. The residue was partitioned between EtOAc (8 mL) and H2O (3 mL). The organic phase was washed with brine, dried (Na2SO4) and concentrated in vacuo to yield a residue. The residue was purified by flash chromatography on silica gel using 20-80% EtOAc in hexanes to give the title compound (300 mg, 53%).
WORKUP
后处理
- customPreparation 2
- temperatureThe mixture was cooled
- concentrationconcentrated in vacuo
- customto yield a residue
- customThe residue was partitioned between EtOAc (8 mL) and H2O (3 mL)
- washThe organic phase was washed with brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated in vacuo
- customto yield a residue
- customThe residue was purified by flash chromatography on silica gel using 20-80% EtOAc in hexanes