Reaction #1442496

ord-f80cede363f34fd493dd113856f90881

Reaction equation

C=CC(=O)OCCC[SiH2]O[Si](C)(C)C
(3-acryloxypropyl)trimethylsiloxy silane
CC(=O)OC=Cc1ccccc1
acetoxystyrene
CC(C)(C#N)N=NC(C)(C)C#N
AIBN
C=CC(=O)OCCC[SiH2]O[Si](C)(C)C.OC=Cc1ccccc1
hydroxystyrene (3-acryloxypropyl)trimethylsiloxy silane

Solvents

Conditions

Temperature
65°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    workup.ADDITIONcharged into a 3-neck flask
  2. 2
    OtherThe system was then purged with N2 for 30 mins before the temperature
  3. 3
    workup.ADDITIONOn the second day, 100 g methanol and 30 mL 30% ammonia hydroxide were added to the system
  4. 4
    Otherwas kept at 60° C
  5. 5
    workup.WAITThe reaction was carried out overnight under N2
  6. 6
    OtherOn the third day, the solution was precipitated in 2000 mL water
  7. 7
    OtherThe polymer was collected
  8. 8
    Otherdried in vacuum oven overnight at 40° C

Procedure

5 g (3-acryloxypropyl)trimethylsiloxy silane, 38 g acetoxystyrene and 2.41 g AIBN were dissolved in 128 g THF and charged into a 3-neck flask. The system was then purged with N2 for 30 mins before the temperature was raised to 65° C. The reaction was carried out overnight under N2. On the second day, 100 g methanol and 30 mL 30% ammonia hydroxide were added to the system and the temperature was kept at 60° C. The reaction was carried out overnight under N2. On the third day, the solution was precipitated in 2000 mL water and 20 mL acetic acid. The polymer was collected and dried in vacuum oven overnight at 40° C. The molecular weight was determined by gel permeation chromatography (GPC) to be 7.5K.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06586156B2uspto-grants-2003_07