Hexane → HCID 13741334, compound

Participants

Reaction Steps

In a three-necked flask, under a nitrogen atmosphere, there were placed 1.22 g (3 mmol) of 4,4′-diiodobiphenyl (product of Tokyo Kasei Kogyo Co., Ltd.), 0.11 g (0.6 mmol) of copper(I) iodide (product of Wako Pure Chemical Industries, Ltd.) and 3.26 g (12 mmol) of cesium carbonate (Wako Pure Chemical Industries, Ltd.). Next, 50 mL of dehydrated toluene (product of Wako Pure Chemical Industries, Ltd.) and 25 mL (9 mmol) of a hexane solution of diphenylphosphine (diphenylphosphine content: 10 mass %, product of Sterm) were added to the flask, and the mixture was heated to reflux for 24 hours. The reaction mixture was then cooled to room temperature and filtered with Celite. After filtration, the solvent was distilled off under reduced pressure and purified by silica gel column chromatography (silica gel, hexane:dichloromethane=2:1), to obtain 650 mg 4,4′-bis(diphenylphosphino)biphenyl represented by the following formula (1) (1.2 mmol, 42% yield), as a phosphine ligand.

Provenance & Evidence