HRID1065533

反应详情

EQUATION

反应方程式

HRID 1065533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In 750 ml. of carbon tetrachloride was dissolved 10 g of 2-fluoro-4-ethylbiphenyl. Then to the solution were added 10 g of N-bromosuccinimide and 0.1 g of benzoyl peroxide. After cooling, a solid substance was filtered off, and from the filtrate containing α-(2-fluoro-4-biphenylyl)ethyl bromide was distilled off the carbon tetrachloride. The residue thus obtained was dissolved in 500 ml. of ethyl alcohol, and then added with 17 g of potassium hydroxide. The resultant mixture was refluxed under heating for 1 hour. After cooling, the reaction mixture was poured into 2.5 l. of water, and then subjected to extraction with benzene. The benzene layer was washed with water, and dried with magnesium sulfate. The benzene in the layer was distilled off, and the resulting residue was subjected to column chromatography. From hexane eluate was obtained 5.5 g of 2-fluoro-4-vinylbiphenyl.

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationa solid substance was filtered off
  3. additionfrom the filtrate containing α-(2-fluoro-4-biphenylyl)ethyl bromide
  4. distillationwas distilled off the carbon tetrachloride
  5. customThe residue thus obtained
  6. dissolutionwas dissolved in 500 ml
  7. temperatureunder heating for 1 hour
  8. temperatureAfter cooling
  9. additionthe reaction mixture was poured into 2.5 l
  10. extractionof water, and then subjected to extraction with benzene
  11. washThe benzene layer was washed with water
  12. dry with materialdried with magnesium sulfate
  13. distillationThe benzene in the layer was distilled off