With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.14871-92-2,(2,2¡ä-Bipyridine)dichloropalladium(II),as a common compound, the synthetic route is as follows.
General procedure: Silver tetrafluoroborate (AgBF4) (0.6 mmol) was dissolvedin methanol (7 mL); (2,2?-bipyridine) dichloropalladium(II)(Pd(Bpy)Cl2) (0.3 mmol) was dissolved in DMSO (1 mL),and then, the solutions were stirred together at ambient temperature0.5 h. Following gravity filtration, solid 3-hydroxyflavonederivative (0.3 mmol) and triethylamine (0.7 mL)were added to the filtrate. The reaction mixture was stirredfor 0.5 h (2 h for the Fla-OMe). The corresponding bipyridinepalladium flavonolato salt was then recovered usingvacuum filtration and recrystallized in CH3OH/CH3CN solvent;remaining solvent was removed in a vacuum desiccatorovernight.[(PdII(Bpy)(3-Hydroxy-4?-methoxyFla)][BF4] complex1 Yield: 129 mg, 70% (orange crystals) Found: C, 50.51;H, 3.01; N, 4.52; Calcd for C26H19BF4N2O4Pd:C, 50.64;H, 3.11; N, 4.54. UV-Vis lambdamax (CH3CN/nm)(epsilon/M-1 cm-1) (444 (25 200); 1H NMR (CD3CN, 400 MHz): delta 7.92 (d,J = 6.5 Hz, 2H), 7.85 (m, J = 21.9 Hz, 4H), 7.65 (t, J = 18.7,2H), 7.47 (d, J = 7.3 Hz, 2H), 7.28 (t, J = 11.4 Hz, 1 H),7.19 (d, J = 6.5 Hz, 2 H), 7.13 (t, J = 13.9 Hz, 1 H), 6.66 (d,J = 8.1 Hz, 2 H); 13C NMR (CD3CN, 400 MHz): delta = 181.44,161.13, 153.96, 153.65, 152.62, 151.82, 150.65, 148.54,148.20, 140.94, 140.67, 138.01, 133.05, 129.37, 129.14,127.34, 127.27, 125.04, 124.44, 124.03, 123.10, 123.01,121.96, 121.73, 117.45, 115.53, 54.91 ppm. ESI MS: m/z(pos.) 529.04.
The synthetic route of 14871-92-2 has been constantly updated, and we look forward to future research findings.
Reference£º
Article; Han, Xiaozhen; Whitfield, Sarah; Cotten, Jacob; Transition Metal Chemistry; (2019);,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method