Réaction #502058

ord-76d56f7fca0d4f9ebb5ec792baae2b6d

Équation de réaction

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

Réactifs

Aucun

Conditions de réaction

Température
100°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

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

Mode opératoire

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)

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08088352B2uspto-grants-2012_01