反应 #1755453

ord-908d8603a3c046dcb19e9e3644ab296f

反应方程式

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

溶剂

反应条件

温度
40°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他To a 1 L reaction flask
  2. 2
    workup.ADDITIONwere added
  3. 3
    其他The reaction vessel was fitted with a mechanical stirrer, condenser
  4. 4
    其他Nitrogen was bubbled through the solution for 15 minutes
  5. 5
    其他to 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
    其他The reactive polymer precipitated
  8. 8
    其他organic solvents were decanted off
  9. 9
    过滤The solid was collected by filtration

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07988988B2uspto-grants-2011_08