Phosphorus pentachloride → Dibutylchlorophosphine

HRID 580365Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 580365
[CH2:1]([PH:5][CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].P(Cl)(Cl)(Cl)(Cl)[Cl:11]>P(Cl)(Cl)Cl>[CH2:1]([P:5]([CH2:6][CH2:7][CH2:8][CH3:9])[Cl:11])[CH2:2][CH2:3][CH3:4]

Komponenten

4

Edukt 2

HCID 24819Phosphorus pentachlorideHCID 74419Phosphine, dibutyl-

Produkt 1

HCID 305896DibutylchlorophosphineAusbeute 55,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 24387Phosphorus trichlorideLösungsmittel

Versuchsvorschrift

148 g (1 mol) di-n-butylphosphine was dropped at a maximum reaction temperature of 30° C. into a suspension of 232 g (1.1 mol) PCl5 in 500 ml toluene. HCl and PCl3 formed during the reaction were removed under a vacuum of 130 mbar and condensed in a cooling trap. After the reaction was complete, the reaction mixture was found to comprise two liquid phases. The upper phase contained PCl3 in toluene. The bulk quantity of chlorophosphine was in the lower phase (31P-NMR). It was worked up distillatively and 101 g product was obtained (55% of the theoretical). bp 92° C./16 mbar.

Aufarbeitung

  1. customformed during the reaction
  2. customwere removed under a vacuum of 130 mbar and condensed in a cooling trap

Quellen und Nachweise

ORD-Eintrag
ord-59cbf71311cf4f3cad9c3b4af5d6e4d9
Quelldatensatz
uspto-grants-1988_06
Patentnummer
US04752648

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