Continuously updated synthesis method about (2,2¡ä-Bipyridine)dichloropalladium(II)

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. 14871-92-2, We look forward to the emergence of more reaction modes in the future.

In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 14871-92-2,(2,2¡ä-Bipyridine)dichloropalladium(II), as follows.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).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. 14871-92-2, We look forward to the emergence of more reaction modes in the future.

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
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