반응 #823763

반응 방정식

HCl MeOH

ethylaluminum sesquichloride

Norbornene

styrene

methyl acrylate

AIBN

Ethylaluminum sesquichloride

→

norbornene styrene methyl acrylate

용매

toluene

toluene

toluene

반응 조건

후처리

1. 1
   workup.WAITthe reaction was performed at 65° C. for 12 hours
2. 2
   기타during the reaction
3. 3
   기타to precipitate a white polymer, which
4. 4
   여과was filtered through a glass
5. 5
   여과filter
6. 6
   기타dried in a vacuum oven at 70° C. for 12 hours

실험 절차

Norbornene (10.5 g, 112 mmol), styrene (0.6 g, 5.6 mmol), methyl acrylate (5 mL, 56 mmol), and AIBN (0.028 g, 0.17 mmol) were charged into a 250 mL Schlenk flask and dissolved in 30 mL of toluene. Ethylaluminum sesquichloride (1.38 g, 5.6 mmol) was charged into a 100 mL flask and dissolved in 20 mL of toluene. The toluene solution of ethylaluminum sesquichloride was slowly dropped to the 250 mL Schlenk flask at −70° C. The reaction temperature was raised to room temperature while stirring the mixture for 2 hours, and then the reaction was performed at 65° C. for 12 hours. The reaction solution turned to light green in color during the reaction. After the reaction was completed, the reaction solution was slowly dropped to 3000 cc of 5% v/v HCl—MeOH to precipitate a white polymer, which was filtered through a glass filter and dried in a vacuum oven at 70° C. for 12 hours to obtain a norbornene-styrene-methyl acrylate terpolymer (7.1 g: 66.7% by weight based on the total weight of used monomers). The copolymer had a Tg of 120° C., a molecular weight (Mw) of 228,000, and Mw/Mn of 16.

출처