Reaction equation
[CH:1]12[CH2:7][CH:4]([CH2:5][CH2:6]1)[CH:3]=[CH:2]2.[C:8]([O:13][CH3:14])(=[O:12])[C:9]([CH3:11])=[CH2:10].CC(N=NC(C#N)(C)C)(C#N)C.CC[Al](Cl)CC.CC[Al](Cl)Cl.Cl.CO>C1(C)C=CC=CC=1>[CH:1]12[CH2:7][CH:4]([CH2:5][CH2:6]1)[CH:3]=[CH:2]2.[C:8]([O:13][CH3:14])(=[O:12])[C:9]([CH3:11])=[CH2:10]Participants
Procedure
Norbornene (8.8 g, 93 mmol), methyl methacrylate (5 mL, 47 mmol), and AIBN (0.23 g, 1.40 mmol) were charged into a 250 mL Schlenk flask and dissolved in 30 mL of toluene. Ethylaluminum sesquichloride (12.7 g, 51.4 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-methyl methacrylate copolymer (0.3 g: 3.0% by weight based on the total weight of used monomers). The copolymer had a Tg of 167° C., a molecular weight (Mw) of 10,700, and Mw/Mn of 3.4.
Workup
- waitthe reaction was performed at 65° C. for 12 hours
- customduring the reaction
- customto precipitate a white polymer, which
- filtrationwas filtered through a glass
- filtrationfilter
- customdried in a vacuum oven at 70° C. for 12 hours
Sources & evidence
- ORD record
- ord-95d961234c0640db929e4f5691aae3d3
- Source dataset
- uspto-grants-2009_09
- Patent number
- US07595369B2
Linked notes
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