Reaktion #1076753

ord-d64aa44f6f2d45baacf37b5781b162f3

Lösungsmittel

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeequipped with a stirrer
  2. 2
    workup.ADDITIONthermometer, addition funnel, and condenser
  3. 3
    TemperaturAfter the temperature had been raised
  4. 4
    Sonstigethe heating mantle was removed
  5. 5
    TemperaturHeat generation
  6. 6
    workup.ADDITIONthe dropwise addition
  7. 7
    Sonstigeexceed 80° C
  8. 8
    workup.ADDITIONAfter the completion of this addition
  9. 9
    SonstigeGas chromatographic analysis of the resulting reaction solution

Vorschrift

123 g (1.1 mol) 1 -octene and 100 microliters of a 2% toluene solution of chloroplatinic acid were placed in a 500-mL four-neck flask equipped with a stirrer, thermometer, addition funnel, and condenser and were heated to 70° C. After the temperature had been raised, the heating mantle was removed and 94.5 g (1 mol) dimethylchlorosilane was added dropwise from the addition funnel. Heat generation was observed immediately, and the dropwise addition was carried out gradually so as to avoid having the temperature of the reaction solution exceed 80° C. After the completion of this addition, the reaction was continued for 30 minutes at 80° C. Gas chromatographic analysis of the resulting reaction solution gave 88% octyldimethylchlorosilane. The reaction solution was cooled to room temperature and 200 g toluene was introduced. The addition funnel was then replaced with a Teflon tube and ammonia was bubbled in until the pH of the reaction solution reached 10. The ammonium chloride product was removed by filtration, and the filtrate was then distillatively purified at 160° C./0.5 mmHg to obtain the following disilazane in a purity of 98 weight %.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06458420B1uspto-grants-2002_10