Tributylamine → 1,1,1-Trichloro-3-vinyl-3,3-dimethyldisiloxane

HRID 1085981

Reaktionsgleichung

Reaktionsgleichung von HRID 1085981
[CH:1]([Si:3]([CH3:11])([CH3:10])[O:4][Si](C=C)(C)C)=[CH2:2].[Cl:12][Si:13]([Cl:16])(Cl)[Cl:14].C(N(CCCC)CCCC)CCC>C(Cl)Cl>[Cl:12][Si:13]([Cl:16])([Cl:14])[O:4][Si:3]([CH:1]=[CH2:2])([CH3:11])[CH3:10]

Komponenten

5

Edukt 3

HCID 7622TributylamineHCID 24816Silicon tetrachlorideHCID 758191,3-Divinyltetramethyldisiloxane

Produkt 1

HCID 200594071,1,1-Trichloro-3-vinyl-3,3-dimethyldisiloxaneAusbeute 114,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture containing 595 g (3.2 mol) of 1,3-divinyl-1,1,3,3-tetramethyldisiloxane, 136 g (0.8 mol) of tetrachlorosilane and 2 ml of a 25% solution of phosphonitrile chloride in methylene chloride is stirred at room temperature for 8 hours. About 2.3 ml of tri-n-butylamine are then added to deactivate the phosphonitrile chloride. The reaction mixture is stirred for 30 minutes and then subjected to fractional distillation. About 216 g of 1,1,1-trichloro-3-vinyl-3,3-dimethyldisiloxane are obtained at 20° to 22° C. and at 2 mbar; about 53 g of 1,5-divinyl1,1,5,5-tetramethyl 3,3-dichlorotrisiloxane are obtained at 23° to 42° C. and at 2 mbar, and 9 g of a 1:1 mixture of 1,5divinyl-1,1,5,5-tetramethyl-3,3-dichlorotrisiloxane and 1,5-divinyl-1,1,5,5-tetramethyl-3-chloro-3-trimethylsiloxytrisiloxane are obtained at 42° to 72° C. and at 2 mbar. About 372 g of vinyldimethylchlorosilane are collected in the cold trap. The desired 1,5-divinyl-1,1,5,5-tetramethyl-3,3-bis(vinyldimethylsiloxy)trisiloxane is not obtained.

Aufarbeitung

  1. stirringThe reaction mixture is stirred for 30 minutes
  2. distillationsubjected to fractional distillation

Quellen und Nachweise

ORD-Eintrag
ord-d76bd27aef1e44ea8f3df94d7593aa54
Quelldatensatz
uspto-grants-1991_04
Patentnummer
US05011962

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