Reaktion #335744

ord-08f010ad8f0a4985ad42f4c7a35b6ff7

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONthe mixture was introduced into a 100 ml bench autoclave
  2. 2
    Sonstigethe autoclave was sealed
  3. 3
    TemperaturThe mixture was warmed at 70° to 80° C. for 90 minutes
  4. 4
    TemperaturThe mixture was then cooled

Vorschrift

About 15.9 g (0.082 Mol) of 4-(5-hexenyl)-1-chlorobenzene were dissolved in 10 ml of toluene, 0.8 ml of a 1 percent solution of dicyclopentadienylplatinum dichloride in dichloromethane (corresponding to 100 ppm of Pt) were added, and the mixture was introduced into a 100 ml bench autoclave. About 10 g (0.147 Mol) of trimethylsilane in the condensed state were added, the autoclave was sealed, and 5 MPa of nitrogen were injected. The mixture was warmed at 70° to 80° C. for 90 minutes (8 MPa, internal stirring). The mixture was then cooled, the solvent was stripped off, and the resultant residue fractionated. About 17.6 g of 4-(1-trimethylsilylhexyl)-1-chlorobenzene, corresponding to 77.1 percent of theory, were obtained at 0.1 hPa and at a boiling range of 107° to 112° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05210247uspto-grants-1993_05