Methyl Acrylate → Norbornene methyl acrylate

HRID 736578

反応式

HRID 736578 の反応式
[CH:1]12[CH2:7][CH:4]([CH2:5][CH2:6]1)[CH:3]=[CH:2]2.[C:8]([O:12][CH3:13])(=[O:11])[CH:9]=[CH2:10].C(OOC(C)(C)C)(C)(C)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:12][CH3:13])(=[O:11])[CH:9]=[CH2:10]

参加物

7

実験手順

Norbornene (15.8 g, 168 mmol), methyl acrylate (10 mL, 112 mmol), and Di-t-butylperoxide (0.32 g, 2.2 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 room temperature while stirring the mixture for 2 hours, and then the reaction was performed at 80° C. for 12 hours. 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 (10.5 g: 52.0% by weight based on the total weight of used monomers). The copolymer had a molecular weight (Mw) of 38,500, and Mw/Mn of 2.29.

後処理

  1. waitthe reaction was performed at 80° C. for 12 hours
  2. customto precipitate a white polymer, which
  3. filtrationwas filtered through a glass
  4. filtrationfilter
  5. customdried in a vacuum oven at 70° C. for 12 hours

出典と根拠

ORDレコード
ord-2ffa5365e83e45568a930c0aaedf1a8e
出典データセット
uspto-grants-2009_09
特許番号
US07595369B2

関連ノート

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