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.
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. 3-(4-(tert-butyl)pyridin-2-yl)-7,8,8-trimethyl-4,5,6,7-tetrahydro-2H-4,7-methanoindazole (70 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 ethyl acetate (hereinafter referred as EA) and n-hexane (EA:n-hexane=1:3 (by volume)). Recrystallization was then conducted using dichloromethane/n-hexane so as to obtain a white crystalline product, referred to as complex E1 (77.4% yield; 137 mg). The reaction scheme for producing the complex E1 is represented as follows: The spectrum analysis for the complex E1 is: 1H NMR (400 MHz, CD2Cl2, 298 K) delta 8.97 (d, J=8.1 Hz, 1H), 7.84 (dd, J=10.4, 18.3 Hz, 4H), 7.38-7.51 (m, 8H), 7.06-7.07 (m, 2H), 6.94 (t, J=7.2 Hz, 1H), 6.47 (dd, J=1.8, 6 Hz, 1H), 3.73 (d, J=11.2 Hz, 2H), 2.97 (d, J=3.7 Hz, 1H), 2.08-2.14 (m, 1H), 1.80-1.86 (m, 1H), 1.43-1.47 (m, 1H), 1.41 (s, 3H), 1.25 (s, 9H), 0.97 (s, 3H), 0.84-0.88 (m, 1H), 0.81 (s, 3H) ppm, 31P NMR (200 MHz, CDCl3, 298 K) delta 36.38 ppm, FAB-MS m/z 779.7 [M+1]+, 7650-91-1
The synthetic route of 7650-91-1 has been constantly updated, and we look forward to future research findings.
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