14871-92-2 A common heterocyclic compound, 14871-92-2,(2,2¡ä-Bipyridine)dichloropalladium(II), its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.
A suspension of 1 mmol (0.333 g) of [Pd(bpy)Cl2] in 150 mL ofacetone was treated with 1 mmol (0.228 g) of benzyl dithiocarbamatesodium salt and the mixture was refluxed under continuousmagnetic stirring for 2 h. Stirring continued for another 12 h at 318 K and then filtered.The resulting yellow colored filtrate containing the desired productwas concentrated to 15 mL at 318 K. The orange precipitate formedwas filtered off and washed with diethyl ether. Recrystallizationwas done by dissolving the precipitate in minimum amount ofethanol. Yield: 0.336 g (70%) and decomposes at 207-209 C. Anal.Calcd. for C18H16N3S2ClPd (480.34 g mol-1) Found, (Calcd.) (%): C45.01, (45.05); H, 3.36 (3.34); N, 8.75 (8.76). Molar conductance forthe complex (10-3 M, H2O) is 9.0 mS m2 mol-1. FT-IR (KBr, cm-1):3405 upsilon(N-H); 3020 upsilon(Caro-H); 1550 upsilon(C-N); 1313 upsilons (CNS); 1036 upsilonas(CNS); 503 upsilon (Pd-N); 450 upsilon (Pd-S). 1H NMR (DMSO-d6-D2O, delta ppm):4.71 (d, 2H, H-c), 7.40 (m,1H, H-a), 7.32 (m, 4H, H-b), 8.54 (m, 2H, H-6,60), 8.27 (m, 2H, H-3,30), 8.18 (m, 2H, H-4,40), 7.68 (M, 2H, H-5,50)(Fig. 1). 13C NMR (DMSO-d6, delta ppm): 48.00 (C-e), 139.67 (C-5,5′),139.84 (C-4,4′), 140.00 (C-a), 140.17 (C-b), 140.34 (C-c), 140.50 (C-3,30), 140.60 (C-d), 140.67 (C-1,10), 140.76 (C-f) (Fig. 1). The NMRnumbering schemes are given in Fig. 1. UV-Vis data (H2O, lambdamax/nm,(log epsilon)): 312 (3.40), 249 (3.75), 187 (3.94).
This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,(2,2¡ä-Bipyridine)dichloropalladium(II),14871-92-2,its application will become more common.
Reference£º
Article; Saeidifar, Maryam; Mirzaei, Hamidreza; Ahmadi Nasab, Navid; Mansouri-Torshizi, Hassan; Journal of Molecular Structure; vol. 1148; (2017); p. 339 – 346;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method