반응 #823762

ord-95d961234c0640db929e4f5691aae3d3

반응 조건

상세 조건
See reaction.notes.procedure_details.

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 (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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07595369B2uspto-grants-2009_09