反応 #823763

ord-dacbc587ff594eefbfdbe450693160b3

反応方程式

CO.Cl
HCl MeOH
C[CH2][Al]([Cl])[CH2]C.C[CH2][Al]([Cl])[Cl]
ethylaluminum sesquichloride
C1=CC2CCC1C2
Norbornene
C=Cc1ccccc1
styrene
C=CC(=O)OC
methyl acrylate
CC(C)(C#N)N=NC(C)(C)C#N
AIBN
C[CH2][Al]([Cl])[CH2]C.C[CH2][Al]([Cl])[Cl]
Ethylaluminum sesquichloride
C1=CC2CCC1C2.C=CC(=O)OC.C=Cc1ccccc1
norbornene styrene methyl acrylate

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.WAITthe reaction was performed at 65° C. for 12 hours
  2. 2
    その他during the reaction
  3. 3
    その他to precipitate a white polymer, which
  4. 4
    ろ過was filtered through a glass
  5. 5
    ろ過filter
  6. 6
    その他dried in a vacuum oven at 70° C. for 12 hours

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07595369B2uspto-grants-2009_09