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

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 hexamethyldisilazene 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.

ORD-Eintrag

ord-ead24a4337c24bf499b405d598d1dd6b

Quelldatensatz

uspto-grants-1996_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05557003