反応 #351009

ord-673df968ccc84d87a1da24d43e9a0ad1

反応方程式

OCCCCCCBr
6-bromo-1-hexanol
CCN(CC)CC
triethylamine
C=CC(=O)Cl
acryloyl chloride
C=CC(=O)OCCCCCCBr
6-bromohexyl acrylate
収率 65.2%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added dropwise
  2. 2
    温度cooling with ice
  3. 3
    workup.STIRRINGstirred for 3 hours
  4. 4
    その他to give a reaction solution
  5. 5
    洗浄The reaction solution was washed with a 3N-HCl
  6. 6
    乾燥with water, dried over sodium sulfate anhydride
  7. 7
    その他the solvent was evaporated
  8. 8
    その他the residue was purified by the silica gel column chromatography (eluent; toluene)

実験手順

Into a reactor, 30 g of 6-bromo-1-hexanol, 18.4 g of triethylamine, and 500 ml of benzene were charged, to which a solution of 16.5 g of acryloyl chloride in 200 ml of benzene was added dropwise, while stirring and cooling with ice, and stirred for 3 hours to give a reaction solution. The reaction solution was washed with a 3N-HCl and then with water, dried over sodium sulfate anhydride, and thereafter the solvent was evaporated and the residue was purified by the silica gel column chromatography (eluent; toluene) to give 25.4 g (Y., 65.1%) of 6-bromohexyl acrylate. GC; 95.9%

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05645760uspto-grants-1997_07