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. 14871-92-2
General procedure: To a stirred suspension of [Pd(bpy)Cl2] (0.03 g, 0.1 mmol) or[Pd(phen)Cl2] (0.04 g, 0.1 mmol) in MeOH (10 mL) a solution ofHhmbt (0.023 g, 0.1 mmol) in MeOH containing KOH (0.006 g,0.1 mmol; 10 mL) was added drop by drop with stirring. The reactionmixture was warmed for 48 h, upon which a yellow-orangeprecipitate was filtered off, washed with MeOH, Et2O and driedin vacuo.For[Pd(bpy)(hmbt)]Cl2H2O: Yield: 0.07 g (51%). ElementalAnal.: Calcd. C, 49.5; H, 4.3; N, 12.6; Pd, 19.1 (C23H24N5O3Pd);Found: C, 49.7; H, 4.2; N, 12.7; Pd, 19.1%. Conductivity data(103 M in DMF): KM = 84.0 ohm1. IR (cm1): m(CN), 1621;m(CO), 1251; m(N-N), 1141; m(Pd-O), 500; m(Pd-N), 459. Raman(cm1): m(CN), 1602; m(CO), 1251; m(N-N), 1141; m(Pd-O), 501;m(Pd-N), 460. 1H NMR (ppm): 8.00 (H(3), d, J = 6 Hz, 1H); 7.75(H(6), S, 1H); 7.86 (H(7), d, J = 5.4 Hz, 1H); 7.73 (H(8), t, J = 5 Hz,1H); 7.69 (H(9), t, J = 5 Hz, 1H); 7.22 (H(10), d, J = 5.2 Hz, 1H);2.50 (CH3, S, 3H). MS (m/z): 486.4 (Calcd. 486.4), 368.2 (Calcd.368.4), 292.4 (Calcd. 292.4), 262.4 (Calcd. 262.4), 156.3 (Calcd.156.0).For[Pd(phen)(hmbt)]ClH2O: Yield: 0.08 g (54%). ElementalAnal.: Calcd. C, 53.2; H, 3.9; N, 12.4; Pd, 18.7 (C25H22N5O2Pd);Found: C, 53.3; H, 4.0; N, 12.3; Pd, 18.6%. Conductivity data(103 M in DMF): KM = 81.0 ohm1. IR (cm1): m(CN), 1600;m(CO), 1252; m(N-N), 1138; m(Pd-O), 564; m(Pd-N), 495. Raman(cm1): m(CN), 1604; m(CO), 1252; m(N-N), 1139; m(Pd-O), 565;m(Pd-N), 495. 1H NMR (ppm): 7.96 (H(3), d, J = 5.1 Hz, 1H); 7.30(H(6), S, 1H); 7.60 (H(7), d, J = 4.5 Hz, 1H); 7.77 (H(8), t,J = 4.2 Hz, 1H); 7.73 (H(9), t, J = 4.5 Hz, 1H); 7.22 (H(10), d,J = 4.2 Hz, 1H); 2.50 (CH3, S, 3H). MS (m/z): 510.4 (Calcd. 510.4),286.4 (Calcd. 286.4), 180.6 (Calcd. 180.0).
This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,14871-92-2,(2,2¡ä-Bipyridine)dichloropalladium(II),its application will become more common.
Reference£º
Article; El-Asmy, Hala A.; Butler, Ian S.; Mouhri, Zhor S.; Jean-Claude, Bertrand J.; Emmam, Mohamed S.; Mostafa, Sahar I.; Journal of Molecular Structure; vol. 1059; 1; (2014); p. 193 – 201;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method