反応 #502058

ord-76d56f7fca0d4f9ebb5ec792baae2b6d

反応方程式

Cc1ccccc1
toluene
O=S(=O)(O)O
sulfuric acid
CCCCO
n-butanol
C=CC(=O)OCCCC
n-Butyl Acrylate

試薬

なし

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他A typical cleavage reaction
  2. 2
    workup.ADDITIONby dispersing 0.1602 g
  3. 3
    その他Solvent was removed by rotary evaporation under reduced pressure
  4. 4
    workup.ADDITIONThe residual solid was dispersed into 100 mL CHCl3
  5. 5
    抽出extracted with water three times
  6. 6
    その他to remove any sulfuric acid
  7. 7
    ろ過The organic dispersion was filtered through a 0.2 μm Nylon membrane
  8. 8
    洗浄washed with CHCl3
  9. 9
    workup.DISTILLATIONThe filtrate was distilled under reduced pressure
  10. 10
    その他to remove the solvent
  11. 11
    その他dried in vacuum overnight at 40° C

実験手順

A typical cleavage reaction was performed by dispersing 0.1602 g GCNF-PBA3 into 100 mL toluene followed by adding 100 mL n-butanol and 5 mL concentrated sulfuric acid and refluxing the mixture at 100° C. for 9 days. Solvent was removed by rotary evaporation under reduced pressure. The residual solid was dispersed into 100 mL CHCl3 and extracted with water three times to remove any sulfuric acid. The organic dispersion was filtered through a 0.2 μm Nylon membrane and washed with CHCl3. The filtrate was distilled under reduced pressure to remove the solvent and dried in vacuum overnight at 40° C. Molecular weight and polydispersity of the cleaved PBA were measured by GPC. (Mw=31,300, Mw/Mn=1.73)

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08088352B2uspto-grants-2012_01