Tetravinylsilane → Tetrakis-(diphenylphosphinoethyl) silane

HRID 544516

Reaktionsgleichung

Reaktionsgleichung von HRID 544516
[CH:1]([Si:3]([CH:8]=[CH2:9])([CH:6]=[CH2:7])[CH:4]=[CH2:5])=[CH2:2].[C:10]1([PH:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>C1(C)C=CC=CC=1>[C:17]1([P:16]([CH2:2][CH2:1][Si:3]([CH2:8][CH2:9][P:16]([C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)([CH2:6][CH2:7][P:16]([C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH2:4][CH2:5][P:16]([C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1

Komponenten

4

Edukt 2

HCID 66188TetravinylsilaneHCID 70017Diphenylphosphine2×

Produkt 1

HCID 54116395Tetrakis-(diphenylphosphinoethyl) silaneAusbeute 39,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

A mixture of 27.2 g (0.2 mole) of tetravinyl silane and 149.5 g (0.804 mole) diphenylphosphine was reacted in a quartz pressure tube at 200° C. with u.v. light initiation until most of the diphenyl phosphine was converted. The hot, molten reaction mixture was added to 720g of hot toluene with stirring. The tetraaduct product precipitated from the solution as a white crystalline solid. The mixture was allowed to coolto ambient temperature and then filtered with suction. After washing with toluene and drying in vacuo, 84 g (47.7%) of crude product was obtained. This was recrystallized from 1200 ml of xylene to obtain 69 g of the pure tetrakis-(diphenylphosphinoethyl) silane of mp. 198°-199° C.

Aufarbeitung

  1. customwas reacted in a quartz pressure tube at 200° C. with u.v
  2. customThe tetraaduct product precipitated from the solution as a white crystalline solid
  3. customto coolto ambient temperature
  4. filtrationfiltered with suction
  5. washAfter washing with toluene
  6. customdrying in vacuo
  7. custom84 g (47.7%) of crude product was obtained
  8. customThis was recrystallized from 1200 ml of xylene

Quellen und Nachweise

ORD-Eintrag
ord-1d831e6dd0de40a7b7c4844939fec56f
Quelldatensatz
uspto-grants-1984_05
Patentnummer
US04450299

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