反応 #1755453

反応方程式

glycidyl methacrylate

Vazo 64

tetrahydrofuran

N,N-dimethylacrylamide

→

DMA GMA

溶媒

ether

反応条件

後処理

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

実験手順

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.

出典