719-80-2,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.719-80-2,Ethoxydiphenylphosphine,as a common compound, the synthetic route is as follows.
To a stirred solution of CsF (63 mg, 0.42 mmol) in anhydrous acetonitrile 1 mL was consecutively added 2,5 dimethyl-(o-trimethyl silyl)phenyl triflate (25 mg, 0.077 mmol) and ethoxydiphenylphosphine (60 mg, 0.31 mmol). Reaction mixture was allowed to stir at room temperature (30 C.) for 30 hrs. The reaction mixture was concentrated and directly loaded on silica gel column and purified by using solvent gradient of Pet. Ether: Ethyl Acetate (1:1) to yield a white solid phosphine oxide (19 mg, 81%). Reaction Time: 30 h; Rf: 0.3 (1:1 EtOAc:Pet Ether); White Solid; mp 157-159 C.; 19.0 mg, 81%; 1H NMR (400 MHz, CDCl3, TMS) delta 7.75-7.60 (m, 4H), 7.59-7.52 (m, 2H), 7.51-7.43 (m, 4H), 7.26-7.20 (m, 1H), 7.19-7.13 (m, 1H), 6.88 (d, J=14.4 Hz, 1H), 2.37 (s, 3H), 2.21 (s, 3H); 13C NMR (100 MHz, CDCl3, TMS) delta 140.0 (d, J=7.7 Hz), 134.7 (d, J=13.1 Hz), 133.9 (d, J=12.3 Hz), 132.9 (d, J=103.3 Hz), 132.8 (d, J=2.3 Hz), 131.9 (d, J=10.0 Hz), 131.8, 131.7 (d, J=3.1 Hz), 130.4 (d, J=103.3 Hz), 128.5 (d, J=11.6 Hz), 21.2 (d, J=4.6 Hz), 21.0; 31P NMR (162 MHz, CDCl3) delta 31.7; HRMS-ESI (m/z) calcd (C20H19OP+H)+: 307.1246 found: 307.1244
719-80-2 Ethoxydiphenylphosphine 69754, achiral-phosphine-ligands compound, is more and more widely used in various fields.
Reference£º
Patent; Mhaske, Santosh Baburao; Dhokale, Ranjeet Ashokrao; US2015/210725; (2015); A1;,
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