반응 #502058

ord-76d56f7fca0d4f9ebb5ec792baae2b6d

반응 방정식

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

시약

없음

반응 조건

온도
100°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타A typical cleavage reaction
  2. 2
    workup.ADDITIONby dispersing 0.1602 g
  3. 3
    기타Solvent was removed by rotary evaporation under reduced pressure
  4. 4
    workup.ADDITIONThe residual solid was dispersed into 100 mL CHCl3
  5. 5
    추출extracted with water three times
  6. 6
    기타to remove any sulfuric acid
  7. 7
    여과The organic dispersion was filtered through a 0.2 μm Nylon membrane
  8. 8
    세척washed with CHCl3
  9. 9
    workup.DISTILLATIONThe filtrate was distilled under reduced pressure
  10. 10
    기타to remove the solvent
  11. 11
    기타dried in vacuum overnight at 40° C

실험 절차

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)

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08088352B2uspto-grants-2012_01