With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.6224-63-1,Tri-m-tolylphosphine,as a common compound, the synthetic route is as follows.
Phosphine 1 (0.22 g, 0.723 mmol) dissolved in EtOH (5 ml) andaq.H2O2 (34%, 0.075 g) was added and resulted mixture was stirredduring 1 h at room temperature. In 1 h MnO2 was added to quenchthe traces of H2O2. Then the mixture was filtered through K2CO3and EtOH was removed in vacuum to give the phosphine oxide 2 aswhite powder.Yield 0.229 g (99%). M.p. 148-150 C (heptane), FTIR (KBr, cm-1):3024, 2921, 2862, 2819, 1922, 1820, 1656, 1599, 1499, 1444, 1399,1310, 1175, 1115, 1025, 807, 660, 523, 464; 1H NMR (400.13 MHz,CDCl3, delta, ppm): 2.35 (Me, 9H, s), 7.16 (3,5-H, C6H4, 6H, br.d,3JHH =7.9 Hz), 7.52 (2,6-H, C6H4, 6H, dd, 3JHH =7.9 Hz,3JPH =11.8 Hz). 13C NMR (100.62 MHz, CDCl3, delta, ppm): 21.55 (Me),129.14 (3,5-C, C6H4, d, 3JPC =12.6 Hz), 129.45 (1-C, C6H4, d,1JPC= 107.5 Hz), 132.10 (2,6-C, C6H4, d, 2JPC =10.4 Hz), 142.21 (4-C,C6H4, d, 4JPC= 2.8 Hz); 31P NMR (161.98 MHz, CDCl3, delta, ppm): 27.49.For C21H21PO calcd (%): , 78.73; , 6.61; , 9.67. Found: , 78.65; ,6.59; , 9.47.
The synthetic route of 6224-63-1 has been constantly updated, and we look forward to future research findings.
Reference£º
Article; Sterkhova; Smirnov; Malysheva; Kuimov; Belogorlova; Journal of Molecular Structure; vol. 1197; (2019); p. 681 – 690;,
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