HRID1969436

反应详情

EQUATION

反应方程式

HRID 1969436 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a mixture of 4-fluorobenzonitrile (2.49 g, 20.6 mmol) and 4-formylpyrazole (1.98 g, 20.6 mmo) in 50 mL of DMF at 0° C. was added 95% sodium hydride (0.54 g, 22.7 mmol) under nitrogen. The mixture was heated to 60° C. for 6 hours and cooled to room temperature. Water was added carefully and the mixture was then extracted with ethyl acetate. The combined extracts were washed with water and brine, and then dried over sodium sulfate, filtered, and concentrated in vacuo to provide crude 4-(4-formyl-1H-pyrazol-1-yl)benzonitrile.

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. extractionthe mixture was then extracted with ethyl acetate
  3. washThe combined extracts were washed with water and brine
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo