With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.109073-77-0,[2,2′-Bipyridine]-4,4′-diyldimethanol,as a common compound, the synthetic route is as follows.
To a solution of [{Ir(mu-Cl)(ptpy)2}2] (169mg, 0.15mmol) in 25mL of a mixture of CH2Cl2/MeOH/H2O (1:1:0.5) the ligand 4,4′-bis(hydroxymethyl-2,2′-bipyridine (65mg, 0.30mmol) was added and the mixture refluxed with stirring for 3h. After cooling to room temperature KPF6 (92mg, 0.50mmol) was added and stirred for 20min. The solvent was removed in vacuo to dryness, the residue dissolved in dichloromethane and chromatographed on alumina with dichloromethane/acetone (9:1) as the eluent. The resulting solution was evaporated to dryness, the residue dissolved in 5mL of dichloromethane and the product was precipitated by slow diffusion with isohexane. (0008) Yield: 104mg (39.1%). Anal. Calc. for C36H32IrN4O2PF6: C, 48.59; H, 3.62; N, 6.30. Found: C, 48.34; H, 3.79; N, 6.46%. MS (FAB+): m/z=745.5 [M+] complex cation. 1H NMR (400MHz, CD2Cl2): delta=8.53 (s, 2H), 7.87(m, 4H), 7.70 (m, 2H), 7.59 (m, 2H), 7.44 (d, J=6.0Hz, 2H), 7.34 (d, J=5.2Hz, 2H), 6.89 (m, 4H), 6.09 (s, 2H), 4.87 (s, 4H), 2.80 (s, br, 2H), 2.11 (s, 6H). 13C{1H} NMR (400MHz, CD2Cl2): delta=167.2, 165.0, 155.8, 154.9, 150.1, 148.5, 141.0, 137.9, 132.4, 125.3, 124.8, 123.6, 122.7, 121.7, 119.4, 62.7 (CH2bpy), 21.5 (Me-ptpy). IR (KBr): nu (cm-1)=3579 w,br, 3395 w,br, 3030 w,br, 2916 w,br, 1609m, 1587m, 1563m, 1480s, 1463m, 1428m, 1418m, 1387 w, 1315 w, 1269 w, 1240 w, 1209 w, 1181 w, 1164 w, 1137 w, 1113 w, 1062 w, 1034 w, 1021 w, 985 w, 845 vs, 774m, 750 w, 739 w, 676 w, 616 w, 558s, 515m, 429 w. UV/vis (nm, M-1 cm-1): 260 (75.200), 274 (78.400), 310 (40.000), 380 (12.000), 408 (7600).
The synthetic route of 109073-77-0 has been constantly updated, and we look forward to future research findings.
Reference£º
Article; Graf, Marion; Siegmund, Daniel; Metzler-Nolte, Nils; Suenkel, Karlheinz; Boettcher, Hans-Christian; Inorganica Chimica Acta; vol. 487; (2019); p. 9 – 14;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI