719-80-2 Ethoxydiphenylphosphine 69754, 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.719-80-2,Ethoxydiphenylphosphine,as a common compound, the synthetic route is as follows.
719-80-2, Under nitrogen, a mixture of 1 (115 mg, 0.138 mmol) and ethyl diphenylphosphinite (600 muL, 2.78 mmol) in a 25 mL flask was heated for 30 min at 100 C. Toluene (2 mL) was then added and the mixture was heated at reflux for 2 h. The product mixture was purified by column chromatography (silica gel) using a non-polar eluent (EtOAc/CH2Cl2, 1:1) to remove by-products and then a polar mixture (EtOAc/MeOH, 9:1) to separate the product. The eluate was concentrated and dried under vacuum to give a white solid foam 2 (175 mg, 95%).1HNMR (400 MHz, CDCl3) delta 7.71-7.66 (m, 12H, Ar-H), 7.50-7.39 (m, 18H, Ar-H),7.04 (dd, 3JHH=7.9 Hz, 4JHP=1.7 Hz, 6H, Ar-H), 6.97 (d, 3JHH = 7.9 Hz, 6H, Ar-H), 4.08 (q, J = 7.1 Hz, 6H, -COCH2CH3),3.65 (d, 2JHP =13.7 Hz, 6H, CH2P(O)Ph2),3.18 (d, J = 15.7 Hz, 6H, ArCHaHb), 2.95 (s,6H, ArCH2-), 2.80 (d, J = 15.7 Hz, 6H, ArCHaHb), 1.18 (t, J = 7.1 Hz, 9H, -COCH2CH3); 13C NMR (100MHz, CDCl3) delta 176.5 (s, -C=O), 136.8 (d, 5JCP = 2.6 Hz, Ar-C), 135.8 (s, Ar-C), 132.6 (d, 1JCP= 97.6 Hz, Ar-C), 132.2 (d, 4JCP = 2.4 Hz, Ar-C), 131.6 (d, 3JCP = 9.2 Hz, Ar-C), 130.4 (d, 3JCP = 4.8 Hz, Ar-C), 130.1 (d, 4JCP = 2.4 Hz, Ar-C), 129.9 (d, 2JCP = 8.0 Hz, Ar-C), 128.9 (d, 2JCP = 11.6 Hz, Ar-C), 61.1, 56.1, 43.7, 40.3, 38.1 (d, 1JCP = 66.2 Hz, CH2P(O)Ph2), 14.1;31P NMR (162 MHz, CDCl3) delta 31.2; HRMS-FAB (NOBA) Calcdfor C84H82O9P3 (M+H+): m/z (rel intensity) 1330.5272 (12.1%),1330.5248 (1.7%), 1329.5239 (40.8%), 1329.5214 (1.8%), 1328.5205 (90.9%),1327.5172 (100.0%),Observed: m/z (relintensity) 1330.5010 (M+4, 16), 1329.5145 (M+3, 44), 1328.5295 (M+2,90),1327.5162 (M+H+, 100), 1277.3716 (11), Elemental analysis: Calcd forC84H81O9P3: C, 76.00; H, 6.15; O,10.85; P, 7.00, Observed: C, 75.78; H, 6.20.
719-80-2 Ethoxydiphenylphosphine 69754, achiral-phosphine-ligands compound, is more and more widely used in various fields.
Reference£º
Article; Lim, Dong Seob; Sahoo, Suban K.; Cho, Chan Sik; Kim, Yang; Choi, Heung-Jin; Tetrahedron Letters; vol. 56; 41; (2015); p. 5665 – 5669;,
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