Triphenylphosphine → 4-Chlorophenyldichlorophosphine

HRID 1249609

Reaktionsgleichung

Reaktionsgleichung von HRID 1249609
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([P:8]([Cl:11])([Cl:10])=O)=[CH:4][CH:3]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([P:8]([Cl:11])[Cl:10])=[CH:4][CH:3]=1

Komponenten

3

Edukt 2

HCID 11776TriphenylphosphineHCID 2724255Phosphonic dichloride, (4-chlorophenyl)-

Produkt 1

HCID 2956054-ChlorophenyldichlorophosphineAusbeute 85 %

Versuchsvorschrift

167 g (0.73 mole) of p-chlorophenylphosphonic acid dichloride and 121 g (0.46 mole) of triphenylphosphane were stirred for 2 hours at 180° C. and for 10 hours at 200° C. under an atmosphere of nitrogen. Distillation was then carried out at 0.04 kPa until a top temperature of 140° C. was reached. This gave 145 g, containing 58.5% of p-chlorophenyldichlorophosphane and 41.5% of p-chlorophenylphosphonic acid dichloride (according to 31P-NMR spectrum). The distillate was fractionated using a 70 cm silvered-jacketed column, packed with Raschig rings. Pure p-chlorophenyldichlorophosphane (boiling point: 71° C./0.093 kPa) was obtained. This corresponds to a yield of 85% of theory, based on triphenylphosphane employed.

Aufarbeitung

  1. distillationDistillation
  2. customwas then carried out at 0.04 kPa until a top temperature of 140° C.
  3. additionThis gave 145 g, containing 58.5% of p-chlorophenyldichlorophosphane and 41.5% of p-chlorophenylphosphonic acid dichloride (according to 31P-NMR spectrum)

Quellen und Nachweise

ORD-Eintrag
ord-0d56a5a8192646eca682f079c80a1fca
Quelldatensatz
uspto-grants-1986_12
Patentnummer
US04632995

Verknüpfte Notizen

Wird geladen…