Reaktion #697895

ord-dac2513f2bcd428bb6e9a1347d9b1ace

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas refluxed for 5 hours
  2. 2
    Sonstigethe solvent removed at atmospheric pressure
  3. 3
    workup.DISTILLATIONdistilled at 67 Pa

Vorschrift

Hydrosilation of diphenylacetylene with bis(dichlorosilyl)trichlorosilylmethane in the presence of H2PtCl6 /IPA. Into the same apparatus as described in Example 1 were placed 0.60 g of diphenylacetylene, 1.06 g of bis(dichlorosilyl)trichlorosilylmethane, 31 μl of 0.1 M H2PtCl6/IPA, and 25 ml of dried benzene forming a mixture. The resulting mixture, with stirring, was refluxed for 5 hours and then the solvent removed at atmospheric pressure. The residue was vacuum distilled at 67 Pa to yield a mixture comprising 1.42 g of 1,1,3,3-tetrachloro-2-trichlorosilyl-4,5-diphenyl-1,3-disilacyclopentane (TCD-GC area 71.2%) and 3,3,5,5-tetrachloro-4-trichlorosilyl-1,2,6,7-tetraphenyl-3,5-disilahepta-1,6-diene (TCD-GC area 5.9%). 1,1,3,3-Tetrachloro-2-trichlorosilyl-4,5-diphenyl- 1,3-disilacyclopentane=1H-NMR (CDCl3, ppm): 1.82 (s, 1H, SiCHSi), 3.35-3.44 (m, 2H, CHPh), 7.06-7.18 (m, 5H, ArH).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05998649uspto-grants-1999_12