تفاعل #502058

ord-76d56f7fca0d4f9ebb5ec792baae2b6d

معادلة التفاعل

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

المتفاعلات

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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)

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08088352B2uspto-grants-2012_01