反応 #823759

ord-3617940dc0354e5db8b6f2a930822d69

反応方程式

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

反応条件

温度
45°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.WAITthe reaction was performed at 45° 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 (15.8 g, 168 mmol), methyl acrylate (10 mL, 112 mmol), and AIBN (2,2′-azobisisobutyronitrile) (0.037 g, 0.22 mmol) were charged into a 250 mL Schlenk flask and dissolved in 30 mL of toluene. Ethylaluminum sesquichloride (0.277 g, 1.12 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 45° C. while stirring the mixture for 2 hours, and then the reaction was performed at 45° 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 acrylate copolymer (11.7 g: 58.2% by weight based on the total weight of used monomers). The copolymer had a Tg of 140° C., a molecular weight (Mw) of 46,600, and Mw/Mn of 1.99.

出典

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