With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.13991-08-7,1,2-Bis(diphenylphosphino)benzene,as a common compound, the synthetic route is as follows.
Under argon atmosphere, silver(I) iodide (235 mg, 1.00 mmol) and 50 mL of the solution of 1,2-bis(diphenylphosphino)benzene (447 mg, 1.00 mmol) in acetonitrile were mixed and the mixture was heated to reflux with stirring for seven hours. The reaction solution was allowed to reach room temperature and the precipitated colorless crystal was filtrated. The obtained filtrated matter was washed with acetonitrile and dried to obtain 531 mg of the complex. The mixture of this complex (49.7 mg) and triphenylphosphine (19.2 mg, 0.0730 mmol) was dissolved in 3 mL of dichloromethane, and the resulting solution was stirred for 30 minutes at room temperature. The reaction solution was concentrated, subjected to recrystallization by slow diffusion of chloroform-diethylether, and dried to provide 30.9 mg of the colorless solid complex. The result of elemental analysis for the obtained complex is shown in Table 2-1, and the composition ratio of the complex was obtained. The present complex corresponds to the above composition formula (3). [Show Image] The NMR data of the obtained complex is provided below. 1H NMR (300 MHz, CDCl3) delta 7.44-7.14 (m, 31H), 7.03 (t, J= 7.2 Hz, 8H); 13C NMR (75 MHz, CDCl3) delta 141.2 (t, J= 22.7 Hz), 134.5 (t, J= 3.0 Hz), 134.2-134.0 (m), 133.3 (d, J= 22.2 Hz), 132.2 (t, J= 10.9 Hz), 129.6 (s), 129.3 (s), 128.5 (d, J= 9.0 Hz), 128.2 (t, J= 4.5 Hz); 31P NMR (122 MHz, CDCl3) delta 3.7 (br, W1/2=159 Hz), -14.8 (br, W1/2 = 450 Hz). The result of DART-MS measurement of the obtained complex is provided below. DART-MS (M/Z): found; 815.16. calcd; 815.13 (M-I)+. Based on the DART-MS measurement of the obtained complex, it was confirmed that the obtained complex contained the following structure.
13991-08-7, As the paragraph descriping shows that 13991-08-7 is playing an increasingly important role.
Reference£º
Patent; Sumitomo Chemical Company, Limited; EP2360162; (2011); 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