反应 #2069929

ord-d7eac201409d43deb09cba2b530eecf4

反应方程式

N#Cc1ccc(-c2ccc(O)cc2)cc1
4-cyano-4′-hydroxybiphenyl
C=CCBr
allyl bromide
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CCC(C)=O
2-butanone
C=CCOc1ccc(-c2ccc(C#N)cc2)cc1
4-allyloxy-4′-cyanobiphenyl
收率 91.3%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他A solution prepared
  2. 2
    温度was refluxed for 7 hours
  3. 3
    洗涤the organic layer was washed with water
  4. 4
    干燥dried with anhydrous magnesium sulfate
  5. 5
    其他The solvent was evaporated away
  6. 6
    其他the resulting residue was purified through silica gel column chromatography
  7. 7
    其他further recrystallized from ethanol

实验过程

A solution prepared by adding 20 g of 4-cyano-4′-hydroxybiphenyl, 20 g of allyl bromide and 25 g of potassium carbonate to 250 ml of 2-butanone was refluxed for 7 hours. Water was added to the reaction solution for liquid-liquid separation, and the organic layer was washed with water and dried with anhydrous magnesium sulfate. The solvent was evaporated away, and the resulting residue was purified through silica gel column chromatography using toluene as an eluent solvent and then further recrystallized from ethanol to obtain 22 g of 4-allyloxy-4′-cyanobiphenyl.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07541071B2uspto-grants-2009_06