Ethanol → HCID 86613233、化合物

HRID 555215ノート

反応式

HRID 555215 の反応式
[C:1]12([CH2:8][CH2:9][Si:10]([O:15][CH3:16])([O:13][CH3:14])[O:11][CH3:12])[CH2:7][CH:4]([CH2:5][CH2:6]1)[CH:3]=[CH:2]2.[CH2:17]([SiH](CC)CC)[CH3:18].C(O)C>ClCCl.C1COCC1.C1(C)C=CC=CC=1>[CH2:8]([C:1]12[CH2:7][CH:4]([CH2:5][CH2:6]1)[CH:3]=[CH:2]2)[CH2:9][CH2:17][CH3:18].[C:1]12([CH2:8][CH2:9][Si:10]([O:15][CH3:16])([O:11][CH3:12])[O:13][CH3:14])[CH2:7][CH:4]([CH2:5][CH2:6]1)[CH:3]=[CH:2]2

参加物

7

反応物 3

HCID 702EthanolHCID 12052TriethylsilaneHCID 22325690[2-(Bicyclo[2.2.1]hept-2-en-1-yl)ethyl](trimethoxy)silane

生成物 1

HCID 86613233HCID 86613233、化合物

試薬・触媒・溶媒 3

HCID 1140Toluene溶媒2 回HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
80 °C

実験手順

BuNB (25.44 g, 0.169 mol), Norbornenylethyltrimethoxysilane (TMSENB, CAS 68245-19-2) (4.56 g, 0.019 mol), triethyl silane (0.11 g, 9.41E-04 mol), ethanol (0.10 g, 2.26E-03 mol) and toluene (170.0 g) were combined in a 300 mL serum bottle and heated to 80° C. in an oil bath to form a solution. To this solution were injected Pd1446 (0.022 g, 1.50E-05 mol) and DANFABA (0.036 g, 4.51E-5 mol), each in the form of a concentrated solution in dichloromethane. After addition, the resulting mixture was maintained at 80° C. for 4 hours. The copolymer was precipitated by adding methanol drop wise into the vigorously stirred reaction mixture. The precipitated copolymer was collected by filtration and dried in an oven at 60° C. under vacuum. After drying, 22.60 g was obtained (69%). The molecular weight of the copolymer was determined by GPC in THF solvent (polystyrene standard) to be Mw=20,000 and Mn=13,000. The composition of the copolymer was determined by 1H-NMR to be (91/9) BuNB/TMSENB copolymer. The refractive indices of this polymer were measured by prism coupling method and determined to be 1.5106 in TE mode and 1.5105 in TM mode at a wavelength of 633 nm. The dried copolymer was dissolved in sufficient toluene to result in a 30 wt % copolymer solution.

後処理

  1. customto form a solution
  2. additionAfter addition
  3. temperaturethe resulting mixture was maintained at 80° C. for 4 hours
  4. customThe copolymer was precipitated
  5. additionby adding methanol
  6. customdrop wise into the vigorously stirred reaction mixture
  7. filtrationThe precipitated copolymer was collected by filtration
  8. customdried in an oven at 60° C. under vacuum
  9. customAfter drying
  10. custom22.60 g was obtained (69%)
  11. customto result in a 30 wt % copolymer solution

出典と根拠

ORDレコード
ord-b83c4687ce724bf595ab649b1982d85f
出典データセット
uspto-grants-2011_11
特許番号
US08053166B2

反応ノート

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