Azobisisobutyronitrile → Norbornene styrene methyl acrylate

Participants

Reaction Steps

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.

Provenance & Evidence