Phosphorus trichloride → Bis(butan-2-yl)(chloro)phosphane

Reaktionsgleichung

[CH3:1][CH:2]([Mg]Cl)[CH2:3][CH3:4].[P:7]([Cl:10])(Cl)Cl>C(OCC)C>[CH3:1][CH:2]([P:7]([CH:2]([CH2:3][CH3:4])[CH3:1])[Cl:10])[CH2:3][CH3:4]

Komponenten

Versuchsvorschrift

In the manner of Examples 6 and 7, 2-butyl magnesium chloride (800 cm3 of a 2M solution in diethyl ether supplied by Aldrich Chemical Co.) was reacted with phosphorus trichloride (110 g) in diethyl ether (450 cm3) to give di-2-butylchlorophosphine (77.8 g, b.p. 84° C. at a pressure of 15 mm of mercury), and this compound was further reacted with hexamethyldisilazane and sulphur to give N-(di-2-butylphosphinothioyl)-P,P-di-2-butylphosphinothioic amide (m.p. 110°-114° C. 31P NMR in CDCl3, multiplet 87.9 ppm downfield of H3PO4). In this compound of Formula I, R1 =R2 =R3 =R4 =2-butyl.