Synthesis
General procedure for the synthesis of 2-(diphenylphosphino)-biphenyl from 2-iodobiphenyl and diphenylphosphine: MCM-41-3N-Pd(0) catalyst (21 mg, 0.01 mmol), KOAc (1.5 mmol), and 2-iodobiphenyl (1.0 mmol if solid) were placed in a 20 mL Schlenk tube that had been pre oven-dried. The reaction vessel was evacuated and displaced three times with argon. Subsequently, 2-iodobiphenyl (1.0 mmol, if liquid), diphenylphosphine (1.2 mmol) and DMAc (1 mL) were added via syringe under argon protection. The reaction mixture was stirred at 130°C for 3 hours. After the reaction was completed, the mixture was cooled to room temperature, diluted with CH2Cl2 (20 mL) and filtered.The MCM-41-3N-Pd(0) catalyst was washed with distilled water (2 × 5 mL) and ethanol (2 × 5 mL) for next use. The filtrate was concentrated under vacuum and the residue was purified by fast column chromatography on silica gel to afford the target product 2-(diphenylphosphino)-biphenyl.
References
[1] Organic Letters, 2003, vol. 5, # 13, p. 2315 - 2318
[2] Applied Organometallic Chemistry, 2018, vol. 32, # 8,
[3] Journal of Organometallic Chemistry, 2018, vol. 866, p. 50 - 58