(OXYDI-2,1-PHENYLENE)BIS(DIPHENYLPHOSPHINE) can be prepared by a one-step reaction of diphenyl ether and diphenylphosphine chloride.
(1) Dilute diphenyl ether (0.02 mol) in hexane (50 mL), add n-BuLi (42 mmol) in hexane solution dropwise at -78 °C (addition completed within about 5 min), react for 1 h, then raise to room temperature (about 25 °C), and continue stirring for 16 h;
(2) Then, 15 mL of a hexane solution of diphenylphosphine chloride (42 mmol) was added dropwise to the reaction system of step (1) under an ice-water bath (the addition was completed within about 5 min), and the reaction was continued to be stirred at room temperature (about 25 °C) for 16 h. The solvent was removed by rotary evaporation, and a pale yellow viscous oily substance was obtained. After washing with acetone and vacuum drying, 9.4 g of white powder was obtained, which was bis(2-diphenylphosphine) ether: yield 87%, 1H NMR (400 MHz, C6D6) δ: 7.41-7.26 (m, 8H, o-PPh2), 7.08-6.93 (m, 14H, m-PPh2, p-PPh2, phenylate), 6.91-6.87 (t, J＝8Hz, 2H, phenylate), 6.72-6.66 (m, 4H, phenylate) ppm.
