Reacción #1755453

ord-908d8603a3c046dcb19e9e3644ab296f

Ecuación de reacción

C=C(C)C(=O)OCC1CO1
glycidyl methacrylate
CC(C)(C#N)N=NC(C)(C)C#N
Vazo 64
C1CCOC1
tetrahydrofuran
C=CC(=O)N(C)C
N,N-dimethylacrylamide
C=C(C)C(=O)OCC1CO1.C=CC(=O)N(C)C
DMA GMA

Disolventes

Condiciones de reacción

Temperatura
40°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroTo a 1 L reaction flask
  2. 2
    workup.ADDITIONwere added
  3. 3
    OtroThe reaction vessel was fitted with a mechanical stirrer, condenser
  4. 4
    OtroNitrogen was bubbled through the solution for 15 minutes
  5. 5
    Otroto remove any dissolved oxygen
  6. 6
    workup.ADDITIONThe reaction mixture was then added slowly to ethyl ether (1.5 L) with good mechanical stirring
  7. 7
    OtroThe reactive polymer precipitated
  8. 8
    Otroorganic solvents were decanted off
  9. 9
    FiltraciónThe solid was collected by filtration

Procedimiento

The DMA/GMA copolymer of Example 13 was prepared by the following procedure. To a 1 L reaction flask were added distilled N,N-dimethylacrylamide (DMA, 48 g, 0.48 moles), distilled glycidyl methacrylate (GMA, 12 g, 0.08 moles) Vazo 64 initiator (AIBN, 0.1 g, 0.0006 moles) and anhydrous tetrahydrofuran (500 ml). The reaction vessel was fitted with a mechanical stirrer, condenser, thermal controller and a nitrogen inlet. Nitrogen was bubbled through the solution for 15 minutes to remove any dissolved oxygen. The reaction flask was then heated to 40° C. under a passive blanket of nitrogen for 168 hours. The reaction mixture was then added slowly to ethyl ether (1.5 L) with good mechanical stirring. The reactive polymer precipitated and organic solvents were decanted off. The solid was collected by filtration and placed in a vacuum oven to remove the ether leaving 58.2 g of reactive polymer (97% yield). The reactive polymer was placed in a desiccator for storage until use.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07988988B2uspto-grants-2011_08