Chlorodiphenylphosphine → HCID 5017640, compound

Participants

Reaction Conditions

Reaction Steps

50 g (0.186 mol) of cylopentadienyl-thallium (obtained from Fluka) together with 300 ml of diethyl ether were placed in a 500 ml flask. The slurry was cooled to 0° C. and 34.2 ml (0.186 mol) of diphenylchlorophosphine were added dropwise over a period of 10 minutes. The slurry was then warmed to room temperature, stirred for one hour and finally filtered through a frit. The solvent was then taken off under reduced pressure and left 39.5 g (85% of the theoretical yield) of the intermediate diphenylphosphino-cyclopentadiene, Compound 5. 18.6 g (0.074 mol) of Compound 5 were then diluted with toluene and cooled to 0° C. 33.2 ml of a 2.24 molar solution of butyl-lithium in hexane (0.074 mol) were added to the above solution over a period of 10 minutes. After warming to room temperature and stirring for 2 hours, the yellow solution gave a precipitate which was filtered off and washed with toluene and subsequently with hexane. Drying under reduced pressure gave 13.2 g of Compound 6 (70% of the theoretical yield) as a brownish powder (cf. J. Am. Chem. Soc. 105 (1983); 3882; Organometallics 1 (1982), 1591).

Provenance & Evidence