Ethanol → HCID 86613233, Verbindung

HRID 1161628Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1161628
[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

Komponenten

7

Edukt 3

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

Produkt 1

HCID 86613233HCID 86613233, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 1140TolueneLösungsmittel2×HCID 6344DichloromethaneLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-514931fc954b46c98287838b1e06af15
Quelldatensatz
uspto-grants-2010_10
Patentnummer
US07820356B2

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