Reaktion #572406

ord-484804a6c0c94b3ea6e8b39d334ae63c

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter the exothermal reaction which
  2. 2
    Sonstigewas terminated
  3. 3
    SonstigeThe yields (31 -P-NMR)
  4. 4
    workup.DISTILLATIONThe crude product was distilled

Vorschrift

19.8 g (0.1 mol) dicyclohexylphosphane was added dropwise at room temperature to 26.1 g (0.11 mol) hexachloroethane. After the exothermal reaction which took place with evolution of HCl was terminated, the reaction mixture was stirred for 3 hours at 100° C. The yields (31 -P-NMR) were as follows: δ P=125.2 ((C6H11)2PCl, 94 wgt %); δ P=194.4 (C6H11PCl2, 2 wgt %); δ P=76.7 ((C6H11)2P(O)Cl, 4 wgt %). The crude product was distilled and 13.7 g (59 wgt %) dicyclohexylchlorophosphane (bp.: 136°-138° C./4 millibars) was obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04536350uspto-grants-1985_08