HRID1804827

反应详情

EQUATION

反应方程式

HRID 1804827 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customPreparation 2
  2. temperatureThe mixture was cooled
  3. concentrationconcentrated in vacuo
  4. customto yield a residue
  5. customThe residue was partitioned between EtOAc (8 mL) and H2O (3 mL)
  6. washThe organic phase was washed with brine
  7. dry with materialdried (Na2SO4)
  8. concentrationconcentrated in vacuo
  9. customto yield a residue
  10. customThe residue was purified by flash chromatography on silica gel using 20-80% EtOAc in hexanes