13991-08-7, 1,2-Bis(diphenylphosphino)benzene is a chiral-phosphine-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
Under argon atmosphere, 20 mL of dry acetonitrile was added to silver(I) bromide (170 mg , 0.904 mmol) and 1,2-bis(diphenylphosphino)benzene (404 mg, 0.904 mmol), and the mixture was stirred at room temperature for one hour and then heated to reflux for seven hours. The reaction solution was allowed to reach room temperature, concentrated, and filtrated after being suspended in 9 mL of chloroform. The filtrated matter was subjected to thermal recrystallization from acetonitrile-chloroform and dried to obtain 399 mg of the colorless crystal complex. Under argon atmosphere, 3 mL of dry dichloromethane was added to the above obtained complex (80.0 mg, 0.0631 mmol) and triphenylphosphine (33.1 mg, 0.126 mmol), and the mixture was stirred at 40C for 10 minutes. The reaction solution was concentrated, subjected to recrystallization by slow diffusion of chloroform-ether, and dried to provide 108 mg of the complex. The result of elemental analysis for the obtained complex is shown in Table 2-2, and the composition ratio of the complex was obtained. The present complex corresponds to the above composition formula (3). The NMR data of the obtained complex is provided below. 1H NMR (300 MHz, CDCl3) delta 7.48-7.17 (m, 31H), 7.07-7.03 (m, 8H); 13C NMR (75 MHz, CDCl3) delta 134.8 (t, J = 2.4 Hz), 134.6-134.2 (m), 130.2-130.0 (m), 129.7 (br), 129.0 (br), 128.9 (br), 128.7-128.6 (m); 31P NMR (122 MHz, CDCl3) delta 8.1 (br, W1/2 = 87 Hz) , -14.8 (br, W1/2 = 340 Hz). The result of DART-MS measurement for the obtained complex is provided below. DART-MS (M/Z): found; 815.16. calcd; 815.13 (M-Br)+. Based on the DART-MS measurement of the obtained complex, it was confirmed that the obtained complex contained the following structure.
13991-08-7, The synthetic route of 13991-08-7 has been constantly updated, and we look forward to future research findings.
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