Ethanol → HCID 21503217, Verbindung

HRID 1287963

Reaktionsgleichung

Reaktionsgleichung von HRID 1287963
[Na].[C:2]1([P:8](Cl)[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:16]([Si:18]([O:25][CH2:26][CH3:27])([O:22][CH2:23][CH3:24])[O:19][CH2:20][CH3:21])=[CH2:17].C([SiH3])=C.C([OH:33])C>C1(C)C=CC=CC=1>[C:2]1([P:8]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)([CH2:17][CH2:16][Si:18]([O:19][CH2:20][CH3:21])([O:25][CH2:26][CH3:27])[O:22][CH2:23][CH3:24])=[O:33])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:9]1([PH:8][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

Komponenten

8

Edukt 5

HCID 702EthanolHCID 6516VinyltriethoxysilaneHCID 66180ChlorodiphenylphosphineHCID 81714VinylsilaneHCID 5360545Sodium

Produkt 2

HCID 70017DiphenylphosphineAusbeute 16,3 %HCID 21503217HCID 21503217, VerbindungAusbeute 16,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

To a suspension of sodium diphenylphosphide prepared, under nitrogen in dry toluene (100 ml), from sodium (4.6, 0.2 g atom) and diphenylphosphinous chloride (22.0 g, 0.1 mol), vinyl triethoxysilane (19.0 g, 0.1 mol) is added during 45 minutes. A slight temperature rise occurs. The temperature is held at 30° C by adjusting the feed rate of the vinyl silane. After 3 hours, 5 ml anhydrous ethanol is added. The yellow color of the anion is instantly discharged. The solution is filtered to remove inorganic salts. Gas chromatographic analysis confirms the presence of diphenyl phosphine and 2-(dipenylphosphinyl)ethyl triethoxysilane. After neutralization with carbon dioxide, the liquid is distilled giving 6.3 g (16.7 percent yield) of 2-(diphenylphosphinyl) ethyl triethoxysilane and 3.0 g (16.3 percent yield) of diphenylphosphine. The H'NMR spectrum of the silane is identical to that of the product of addition of diphenylphosphine to vinyl triethoxysilane with a radical initiator.

Aufarbeitung

  1. additionis added during 45 minutes
  2. customis held at 30° C
  3. filtrationThe solution is filtered
  4. customto remove inorganic salts
  5. distillationAfter neutralization with carbon dioxide, the liquid is distilled

Quellen und Nachweise

ORD-Eintrag
ord-3a1a5d85b97544fc8c317f13b16ea707
Quelldatensatz
uspto-grants-1976_10
Patentnummer
US03987009

Verknüpfte Notizen

Wird geladen…