Month: September 2020

A common heterocyclic compound, (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

[Pd(bpy)Cl2] (.67 g, 2 mmol) was suspended in 200 mlacetone-water (3:1 v/v) and AgNO3 (.68 g, 4 mmol) wasadded with constant stirring. This mixture was heated at328 K with stirring in the dark for 6 h followed by stirringfor 16 h at room temperature. The AgCl precipitatewas removed by filtration using Whatman 42 filter paper.The clear yellow filtrate was mixed with mu-paraxylidinebisdithiocarbamatedisodium salt (.33 g, 1 mmol).The reaction mixture was subsequently stirred for 5 h at318 K and then filtered. The clear solution was concentratedto 5 ml at 318 K. The resulting yellow precipitatewas filtered and washed with small amounts of acetoneand resolved in 300 ml doubly distilled water at 318 K.The solution was filtered to remove turbidity. The clearsolution was then concentrated to 5 ml and refrigeratedovernight. The yellow precipitate was filtered and washedwith small amounts of cold distilled water and acetoneand dried in an oven at 318 K. The synthesis of the complexcan be summarized by Figure 1. Yield: .572 g(65%), Decomposition ranges: 520-523 K. Anal. Calcd.for C30H26N6S4Cl2Pd2: C, 40.86; H, 2.95, N, 9.53%.Found: C, 40.85; H, 2.96, N, 9.55%. Molar conductance,LambdaM (H2O, Omega-1 mol-1 cm2): 243. FT-IR (KBr pellets,cm-1): 1541 upsilon (C-N); 1022 upsilon (C-S) and 1385 (NO3- ion).UV-Vis data (water, lambdamax/nm (logepsilon): 308 (3.43), 247 (3.79) and 188 (3.95). 1H NMR (500 MHz, DMSO-d6,ppm, d = doublet, t = triplet and m = multiple): 7.66 (m,1H, H-a), 8.23 (m, 2H, H-b), 8.48 (d, 2H, H-c), 7.79(t, 2H, H-5,5), 8.30 (t, 2H, H-4,4), 8.57 (d, 2H, H-3,3),8.88 (d, 2H, H-6,6) (Figure S1).

The chemical industry reduces the impact on the environment during synthesis,14871-92-2,(2,2¡ä-Bipyridine)dichloropalladium(II),I believe this compound will play a more active role in future production and life.

Reference£º
Letter; Saeidifar, Maryam; Sohrabi Jam, Zahra; Shahraki, Somayeh; Khanlarkhani, Ali; Javaheri, Masoumeh; Divsalar, Adeleh; Mansouri-Torshizi, Hassan; Akbar Saboury, Ali; Journal of Biomolecular Structure and Dynamics; vol. 35; 12; (2017); p. 2557 – 2564;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

(2,2¡ä-Bipyridine)dichloropalladium(II), A common heterocyclic compound, 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: Palladium(II) chloride (PdCl2), 2,2?-bipyridine (bipy), 1,10-phenanthroline (phen), thiourea (TU, 1), N-methylthiourea (meTU, 2), N-buthylthiourea (buTU, 3), N,N?-diethylthiourea (dietTU, 4) and N,N?-dibuthylthiourea (dibuTU, 5) were purchased as pure reagents at AG, from Sigma Aldrich. Potassium tetrachloropalladate(II) was prepared by the reaction of palladium chloride with a slight excess of potassium chloride. The complexes [Pd(bipy)Cl2] and [Pd(phen)Cl2], were obtained by adding 1 mmol of the respective ligand to 0.326 g (1 mmol) of K2[PdCl4] suspended/dissolved in 40 mL of wet methanol under reflux for about 1 h. The precipitated crystalline powders were recovered by filtration and dried under vacuum for 2 h. 0.25 mmol of these complexes (83 and 89 mg, respectively) were then suspended again in a water/methanol mixture, whereupon 0.5 mmol of the respective thiourea (1-5) was added under reflux. After 1 h, clear yellow to orange solutions were obtained. These solutions were filtrated and the filtrates were kept for 3-5 days at room temperature for crystallization. As a result yellow-red crystals were obtained. The experimental yield of the products, based on Pd, was more than 50%. All the solvents, of analytical grade, were dried and deoxygenated before being used. Elemental analyses were performed at the Microanalytical Laboratory of Redox snc (Milano). Characterization details are extensively quoted in the supplementary material.

14871-92-2 is used more and more widely, we look forward to future research findings about (2,2¡ä-Bipyridine)dichloropalladium(II)

Reference£º
Article; Rotondo, Archimede; Barresi, Salvatore; Cusumano, Matteo; Rotondo, Enrico; Polyhedron; vol. 45; 1; (2012); p. 23 – 29;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

A common heterocyclic compound, (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

[Pd(bpy)Cl2] (0.20 g, 0.60 mmol) was suspended in water (25 mL). Silver nitrate (0.20 g, 1.19 mmol) in water (5 mL) was added and the reaction mixture was stirred for 6 h at 60 C and then at room temperature, always in absence of light. The resulting solution was centrifuged and filtered to remove AgCl. A few drops of water, glycolic acid (0.05 g, 0.66 mmol) and 1 M NaOH (1.20 mL) were added to the filtrate. The resulting solution was stirred for 5 days and concentrated at 60 C to 5 mL on a rotary evaporator. The mixture was cooled to room temperature and the yellow powder was filtered off and dissolved from water and again concentrated to 5 mL. Yellow single crystals suitable for X-ray diffraction were obtained from the resulting solution by slow evaporation at room temperature. Yield: 41%, m.p.: 212 C. Elemental Anal. Calc. for C12H16N2O6Pd (390.67): C, 36.9; H, 4.1; N, 7.2. Found: C, 36.7; H, 4.0; N, 7.1%. MS (FAB+): m/z [assignment(relative intensity)]: 337(35) [M+], 262(94), 157(100). IR (KBr, numax/cm-1): 3376 m,br, 3207 m,br, nu(OH); 1626 s, nu(CC), nuasym(CO2); 1497 w, 1451 m, nu(CC,CN); 1370 m, nusim(CO2); 415 m. Far-IR (Nujol, numax/cm-1): 385 s, nu(Pd-O); 252 m, nu(Pd-N). 1H NMR (CD3OD, delta/ppm): 4.35 (s, 2H, b), 7.71 (m, 2H, 5,5?), 8.28 (m, 2H, 4,4?), 8.39 (d, 2H, 3,3?), 8.49 (d, 2H, 6,6?). 13C NMR (CD3OD, delta/ppm): 72.71 (1C, b), 124.93 (2C, 3,3?), 128.64, 129.04 (2C, 5,5?), 142.44, 142.78 (2C, 4,4?), 150.10, 151.44 (2C, 6,6?). UV-Vis (numax/cm-1): 36101, 30120, 26525 (Reflectance).

The chemical industry reduces the impact on the environment during synthesis,14871-92-2,(2,2¡ä-Bipyridine)dichloropalladium(II),I believe this compound will play a more active role in future production and life.

Reference£º
Article; Balboa, Susana; Carballo, Rosa; Castineiras, Alfonso; Gonzalez-Perez, Josefa Maria; Niclos-Gutierrez, Juan; Polyhedron; vol. 50; 1; (2013); p. 512 – 523;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

(2,2¡ä-Bipyridine)dichloropalladium(II), A common heterocyclic compound, 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

(bpy)PdCl2 (167 mg, 0.5 mmol) and AgNO3 (170 mg, 1.0 mmol) was mixed in CH3NO2 (40 mL). The mixture was stirred at 60 C for 24 hrs, and the white AgCl precipitate was filtered by a short pad of celite. The filtrate was sampled for ESI-HRMS, and cationic C20H18N4O2Pd22+ (m/z: 279.9743) was observed. Then the filtrate was concentrated and recrystallized to give 25 mg light yellow needle-like solid. Yield 9.0%.

14871-92-2 is used more and more widely, we look forward to future research findings about (2,2¡ä-Bipyridine)dichloropalladium(II)

Reference£º
Article; Yang, Zhenyu; Ni, Yuxin; Liu, Rui; Song, Kaixuan; Lin, Shaohui; Pan, Qinmin; Tetrahedron Letters; vol. 58; 21; (2017); p. 2034 – 2037;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact.52522-40-4, Tris(dibenzylideneacetone)dipalladium-chloroform it is a common compound, a new synthetic route is introduced below.52522-40-4

Stage 2: Stage 1 material (8.50 g) and 3,5-bis(4-tert-butylphenyl)phenyl-1-boronic acid pinacol ester (15.50 g) were dissolved in toluene (230 mL). The solution was purged with nitrogen for 1 h before 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (66 mg) and tris(dibenzylidene)dipalladium (75 mg) were added using 10 mL of nitrogen-purged toluene. A 20wtpercent solution of tetraethylammonium hydroxide in water (60 mL) was added in one portion and the mixture as stirred for 20 h with the heating bath set to 105 ¡ãC. T.L.C. analysis indicated all the stage material had been consumed and only one fluorescent spot was observed. The reaction mixture was cooled and filtered into a separating funnel. The layers were separated and the aqueous layer extracted with toluene. The organic extracts were washed with water, dried with magnesium sulphate, filtered and concentrated to yield the crude product as a yellow/orange solid. Pure compound was obtained by column chromatography eluting with a gradient of ethyl acetate in hexanes followed by precipitation from DCM/methanol. HPLC indicated a purity of 99.75percent and a yield of 80percent (11.32g). 1H NMR (referenced to CDCl3): 7.83 (3H, d), 7.76 (6H, s), 7.73 (3H, s) 7.63 (12H, d) 7.49 (12H, d), 7.21 (3H, dd), 6.88 (3H, d), 4.28 (9H, s), 2.25 (3H, m), 1.98 (3H, m), 1.4-1.5 (57H, m), 1.23 (3H, m), 0.74 (9H, t)

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand Tris(dibenzylideneacetone)dipalladium-chloroform reaction routes.

Reference£º
Patent; Cambridge Display Technology Limited; Sumitomo Chemical Co., Ltd; Kamtekar, Kiran; Steudel, Annette; EP2738195; (2014); A1;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

Tris(dibenzylideneacetone)dipalladium-chloroform, A common heterocyclic compound, 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.”52522-40-4

General procedure: To 64.3 mg (0.278 mmol) of TTbQ-Me dissolved in anhydrous acetone (20 ml) in a two necked flask, 30 mg (0.278 mmol) of p-benzoquinone and 120 mg (0.116 mmol) of Pd2DBA3CHCl3 were added in sequence under inert atmosphere (Ar). The resulting mixture was stirred in the dark for 30 min, filtered on a celite filter and evaporated under vacuum to a small volume. Addition of Et2O induces the precipitation of the complex which was filtered off and dried in a desiccator for 5 h. 82.2 mg of the title compound as a red solid were obtained (yield 80percent).

52522-40-4 is used more and more widely, we look forward to future research findings about Tris(dibenzylideneacetone)dipalladium-chloroform

Reference£º
Article; Canovese, Luciano; Visentin, Fabiano; Santo, Claudio; Bertolasi, Valerio; Journal of Organometallic Chemistry; vol. 749; (2014); p. 379 – 386;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

14871-92-2, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact.14871-92-2, (2,2¡ä-Bipyridine)dichloropalladium(II) it is a common compound, a new synthetic route is introduced below.

To a yellow suspension containing 0.30 g (0.90 mmol) of [Pd(bpy)Cl2] in water (20 mL) wereadded a solution containing 0.06 g (0.46 mmol) of HaptHCl in water (10 mL) and an aqueoussolution of NaOH (0.3 M, 10 mL). When the mixture was stirred at 50 C for 3 h, the suspensionturned to a yellow solution. After filtration, a saturated aqueous solution of NaNO3 (10 mL) wasadded to the yellow filtrate, followed by storing in a refrigerator for 1 week. The resulting yellowcrystals of [3](NO3)2 suitable for X-ray analysis were collected by filtration. Yield: 0.19 g (55%).

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; Kouno, Masahiro; Miyashita, Yoshitaro; Yoshinari, Nobuto; Konno, Takumi; Chemistry Letters; vol. 44; 11; (2015); p. 1512 – 1514;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

A common heterocyclic compound, (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).

The chemical industry reduces the impact on the environment during synthesis,14871-92-2,(2,2¡ä-Bipyridine)dichloropalladium(II),I believe this compound will play a more active role in future production and life.

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

52522-40-4, A common heterocyclic compound, 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.”52522-40-4

tetrakis(triphenylphosphine)palladium(0) [generated in situ from tris(diphenylmethylideneacetone)dipalladium chloroform adduct (16 mg, 0.016 mmol) and triphenylphosphine 312 mg, 0.12 mmol)] ; tetrakis(triphenylphosphine)palladium (0) [generated in situ from tris(dibenzylideneacetone)dipalladium chloroform adduct (27 mg, 0.025 mmol) and triphenylphosphine (52 mg, 0.20 mmol)]

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand Tris(dibenzylideneacetone)dipalladium-chloroform reaction routes.

Reference£º
Patent; Universitetet i Olso; US2007/203159; (2007); A1;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact.52522-40-4, Tris(dibenzylideneacetone)dipalladium-chloroform it is a common compound, a new synthetic route is introduced below.52522-40-4

The catalyst was prepared according to the reported procedure in the literature [36], which briefly will explain here. A solution containing Pd2(dba)3.CHCl3 (0.149g, 0.15mmol) and Pt(Ph2Ppy)2Cl2 (0.237g, 0.30mmol) in 50mL of dichloromethane was heated in reflux condition for 2h under nitrogen atmosphere. Then the solution was cooled to room temperature, and diethyl ether was added slowly to precipitate a greenish brown solid. The precipitate was collected by filtration and dried by vacuum. Yield 0.085g, 73percent. C34H28Cl2N2P2PdPt (MW=898.95): calcd. C 45.43, H 3.14, N, 3.12. Found: C 45.21, H 3.13, N 3.48. 1H NMR in CDCl3: delta 9.61?9.50 (m, 2H), 7.75?7.32 (m, 24H), 6.78?6.67 (m, 2H). 31P NMR in CDCl3: delta?7.6 (d, 3JPaPb=14Hz, 1JPtP=4047Hz, 1P, Pa bonded to the Pt), 32.4 (d, 3JPaPb=14Hz, 1JPtP=111Hz, 1P, Pb bonded to the Pd) ppm.

As the rapid development of chemical substances, we look forward to future research findings about 52522-40-4

Reference£º
Article; Gholinejad, Mohammad; Shahsavari, Hamid R.; Razeghi, Mehran; Niazi, Maryam; Hamed, Fatemeh; Journal of Organometallic Chemistry; vol. 796; (2015); p. 3 – 10;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method