With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.7650-91-1,Benzyldiphenylphosphine,as a common compound, the synthetic route is as follows.
7650-91-1, Pt(tht)2Cl2 (synthesized according to a method disclosed in J. Chem. Soc., Dalton Trans. 1980, 888-894; 100 mg, 1 eq, ?tht? represents tetrahydrothiophene), benzyldiphenylphosphine purchased from Alfa Aesar (68 mg, 1.1 eq), and sodium acetate (94 mg, 5 eq) were added in a 50 mL round-bottomed flask, and degassed xylene (purchased from ECHOChemical; Product no: XA2101-000000-72EC; 6 mL) was then added therein with mixing to obtain a mixture, followed by heating to 100 C. and reacting for 12 hours. The mixture was then cooled to room temperature, and a precursor solution (PS1) of a phosphorescent four-coordinated platinum (II) complex was obtained. 4-(tert-butyl)-2-(3-trifluoromethyl-1H-pyrazol-5-yl)pyridine (61 mg, 1 eq) was added into the PS1 obtained from Synthesis Example 1 to obtain a mixture, and the mixture was heated to 100 C. and reacted for 6 hours, followed by cooling to room temperature and removing the solvent. Silica-gel column chromatography was conducted to purify the mixture using an eluent of dichloromethane and n-hexane (dichloromethane:n-hexane=1:1 (by volume)). Recrystallization was then conducted using dichloromethane/n-hexane so as to obtain a light yellow crystalline product, referred to as complex E5 (60.8% yield; 102 mg). The reaction scheme for producing the complex E5 is represented as follows: The spectrum analysis for the complex E5 is: 1H NMR (400 MHz, CDCl3, 298 K) delta 8.89 (d, J=8.3 Hz, 1H), 7.83 (dd, J=8.1, 11.7 Hz, 4H), 7.61 (d, J=1.4 Hz, 1H), 7.56 (d, J=6.1 Hz, 1H), 7.42-7.51 (m, 6H), 7.11 (t, J=6.4 Hz, 2H), 6.98 (t, J=7.4 Hz, 1H), 6.94 (s, 1H), 6.64 (dd, J=2.1, 6.1 Hz, 1H), 3.77 (d, J=11.4 Hz, 2H), 1.26 (s, 9H), 19F NMR (400 MHz, CDCl3, 298 K) delta -60.7, 31P NMR (200 MHz, CDCl3, 298 K) delta 36.24, FAB-MS m/z 738.7 M+
7650-91-1 Benzyldiphenylphosphine 603920, achiral-phosphine-ligands compound, is more and more widely used in various fields.
Reference£º
Patent; National Tsing Hua University; Chi, Yun; Huang, Li-Min; US8722885; (2014); B1;,
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