Analyzing the synthesis route of 166330-10-5

166330-10-5 (Oxybis(2,1-phenylene))bis(diphenylphosphine) 4285986, achiral-phosphine-ligands compound, is more and more widely used in various fields.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.166330-10-5,(Oxybis(2,1-phenylene))bis(diphenylphosphine),as a common compound, the synthetic route is as follows.

General procedure: NHC-Cu(I) complexes 1-3 were synthesized by the following route:a solution of imidazolium salt (0.4 mmol), copper powder (0.12 g,0.5 mmol) and POP (0.64 g, 1.2 mmol) reacted in CH3CN (5 mL) at 50Cfor 12 h. The resulting mixture was filtered through a plug of Celite andconcentrated to ca. 1 mL. Addition of Et2O (10 ml) to the filtrate affordeda pale yellow precipitate, which was collected and washed withEt2O. And the product was recrystallized with ethanol.2.2.6. [Cu(Ph-BenIm-methPy)](PF6) (1)The product was a white powder. Yield: 0.67 g, 67%. 1H NMR(400 MHz, DMSO-d6): delta 8.25 (d, J =8.3 Hz, 1 H), 8.20 – 8.05 (m, 2 H),7.48 (t, J =7.2 Hz, 1 H), 7.34 (t, J =7.7 Hz, 9 H), 7.22 (dd, J=18.7,7.0 Hz, 9 H), 7.06 (dt, J=26.2, 7.6 Hz, 11 H), 6.92 (s, 4 H), 6.78 (s,2 H), 6.72 (d, J =7.4 Hz, 2 H), 5.36 (s, 2 H), 1.90 (d, J =23.9 Hz, 3 H).13C NMR (101 MHz, DMSO-d6). delta 158.85, 157.42, 157.37, 157.31,149.91, 140.91, 134.83, 134.73, 133.63, 132.93, 132.29, 131.54,131.38, 131.23, 130.14, 128.76, 128.59, 127.55, 125.85, 125.08,124.68, 124.54, 123.73, 123.59, 123.46, 122.98, 119.86, 113.33,112.59, 111.80, 51.57, 24.16. 31P NMR (162 MHz, DMSO) delta -10.31 (s),-143.84 (quint). HRMS (m/z, ESI+): calcd. For C56H45CuN3OP2 ([M]+)900.2334; found 900.2358. Anal. Calcd. For C56H45CuF6N3OP3(1045.4): C 64.28, H 4.33, N 4.02; found: C 64.51, H 4.22, N 4.09., 166330-10-5

166330-10-5 (Oxybis(2,1-phenylene))bis(diphenylphosphine) 4285986, achiral-phosphine-ligands compound, is more and more widely used in various fields.

Reference£º
Article; Wang, Jinglan; Chen, Hongyun; Xu, Shengxian; Su, Qingzhi; Zhao, Feng; He, Haifeng; Journal of Photochemistry and Photobiology A: Chemistry; vol. 387; (2020);,
Phosphine ligand
Chiral phosphine ligands in asymmetric synthesis. Molecular structure and absolute configuration of (1,5-cyclooctadiene)-(2S,3S)-2,3-bis(diphenylphosphino)butanerhodium(I) perchlorate tetrahydrofuran solvate