HRID2184909

反应详情

EQUATION

反应方程式

HRID 2184909 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-(2-bromoacetyl)benzonitrile (500 mg, 2.23 mmol) in 5 ml dichloromethane was added pyrazole (304 mg, 4.46 mmol) and triethylamine (0.31 ml, 2.23 mmol). Reaction was stirred at room temperature over night. Reaction was then diluted with 20 ml dichloromethane, washed with 2×25 ml water, 2×25 ml 1N HCl, dried over magnesium sulfate, filtered and concentrated in vacuo. Crude residue was chromatographed on silica gel using 2.5% EtOAc in hexane to give 3-[2-(1H-1-pyrazolyl)acetyl]benzonitrile (330 mg, 70%) as a clear oil after drying. ES-MS (M+H+): 212.05

WORKUP

后处理

  1. customReaction
  2. customReaction
  3. washwashed with 2×25 ml water, 2×25 ml 1N HCl
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customCrude residue was chromatographed on silica gel using 2.5% EtOAc in hexane