Ethanol → 5-Norbornene 2-allylacetate 5-butylnorbornene
反応式
[CH:1]12[CH2:7][CH:4]([CH:5]=[CH:6]1)[CH2:3][CH2:2]2.[CH2:8]([CH2:11][C:12]([O-:14])=[O:13])[CH:9]=[CH2:10].[CH2:15]([CH:19]1[CH2:24][CH:23]2[CH2:25][CH:20]1[CH:21]=[CH:22]2)[CH2:16][CH2:17][CH3:18].C1(C)C=CC=CC=1.C(O)C>C(Cl)Cl.CC([O-])=O.CC([O-])=O.[Pd+2]>[CH:1]12[CH2:7][CH:4]([CH:3]=[CH:2]1)[CH2:5][CH2:6]2.[CH2:8]([CH2:11][C:12]([O-:14])=[O:13])[CH:9]=[CH2:10].[CH2:15]([CH:19]1[CH2:24][CH:23]2[CH2:25][CH:20]1[CH:21]=[CH:22]2)[CH2:16][CH2:17][CH3:18]参加物
反応条件
- 温度
- 90 °C
実験手順
5-norbornene-2-allylacetate (NB—CH2—O—C(O)—CH3) (5 mL, 30.9 mmol), 5-butylnorbornene (1.3 mL, 7.7 mmol), and toluene (7.3 mL) were charged into a 250 mL Schlenk flask. Pd(OAc)2 (0.17 mg, 0.77 p mol) and [(Cy)3PH][(B(C6F5)4) (1.48 mg, 1.55 p mol) were dissolved in CH2Cl2 (1 mL) and added to the monomer solution. While the reaction mixture was stirred for 18 hours at 90° C., the reaction mixture became viscous. After the reaction was completed, 120 ml of toluene was added to the viscous solution to dilute it. The solution was poured into an excess of ethanol to precipitate a white polymer, which was filtered through a glass funnel, washed with ethanol, and dried in vacuo at 80° C. for 24 hours to yield 5-norbornene-2-allylacetate/5-butylnorbornene copolymer (4.35 g: 69.2% by weight based on the total weight of used monomers). The weight average molecular weight (Mw) of the copolymer was 303,550 and Mw/Mn was 2.16.
後処理
- additionadded to the monomer solution
- additionto dilute it
- customto precipitate a white polymer, which
- filtrationwas filtered through a glass funnel
- washwashed with ethanol
- customdried in vacuo at 80° C. for 24 hours
出典と根拠
- ORDレコード
- ord-d61723dacc474dc480954dcbdb26e9bd
- 出典データセット
- uspto-grants-2010_10
- 特許番号
- US07814713B2
反応ノート
読み込み中…