反応 #5123

ord-603826e869b34924b60f03525d155479

反応方程式

Cc1cccc(CCl)c1
3-methylbenzyl chloride
C=CC(=O)OCC
ethyl acrylate
CCC[CH2][SnH]([CH2]CCC)[CH2]CCC
tri-n-butyltin hydride
CCOC(=O)CCCc1cccc(C)c1
ethyl-4-(3-methylphenyl)butanoate

反応条件

温度
110°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwhich was added to the above mixture over a period of 2 hours
  2. 2
    温度This reaction mixture was further heated at the boiling temperature for 2 hours
  3. 3
    温度cooled to the ambient temperature
  4. 4
    その他The residues obtained
  5. 5
    その他after removing the solvent from the mixture
  6. 6
    その他were purified by silica gel column chromatography

実験手順

A mixture of 14.0 g of 3-methylbenzyl chloride and 50.0 g of ethyl acrylate dissolved in 300 ml of dry toluene was heated to 110° C. Separatively, 3.0 g of 2,2'-azobisisobutyronitrile(AIBN) and 32.0 g of tri-n-butyltin hydride were dissolved in 200 ml of dry toluene, which was added to the above mixture over a period of 2 hours. This reaction mixture was further heated at the boiling temperature for 2 hours and then cooled to the ambient temperature. The residues obtained after removing the solvent from the mixture were purified by silica gel column chromatography to provide ethyl-4-(3-methylphenyl)butanoate.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05242944uspto-grants-1993_09