反应 #502058

ord-76d56f7fca0d4f9ebb5ec792baae2b6d

反应方程式

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

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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)

来源

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