HRID1064263

反应详情

EQUATION

反应方程式

HRID 1064263 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5′-Acetyl-2′-fluorobiphenyl-2-carbonitrile (0.31 g, 1.3 mmol) was suspended in 1,4-dioxane (4.75 ml) and water (0.25 ml) and warmed to 60° C. to solubilise the starting material. The solution was then cooled to ambient temperature, selenium dioxide (0.17 g, 1.55 mmol) added and the mixture heated under reflux for 2 h. The mixture was then allowed to cool to 60° C., activated charcoal (1 g) added and the mixture stirred for 30 min. The mixture was then allowed to cool to ambient temperature, filtered through a glass fibre filter paper and the solid washed with 1,4-dioxane (10 ml) and the filtrate evaporated to give crude 2′-fluoro-5′-(2-oxoacetyl)biphenyl-2-carbonitrile which was used without further purification in the next step.

WORKUP

后处理

  1. temperaturethe mixture heated
  2. temperatureunder reflux for 2 h
  3. temperatureto cool to 60° C.
  4. temperatureto cool to ambient temperature
  5. filtrationfiltered through a glass fibre
  6. filtrationfilter paper
  7. washthe solid washed with 1,4-dioxane (10 ml)
  8. customthe filtrate evaporated