Month: November 2020

14871-92-2,Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. (2,2¡ä-Bipyridine)dichloropalladium(II),14871-92-2, This compound has unique chemical properties. The synthetic route is as follows.

Synthesis of [Pd{OC(O)CH2N(COPh)}(bipy)] 2 A mixture of [PdCl2(bipy)] (210 mg, 0.63 mmol) with hippuric acid (113 mg, 0.63 mmol) and silver(I) oxide (600 mg) in dichloromethane (30 mL) was refluxed for 3.5 h. Methanol (30 mL) was added, and the mixture filtered to give a clear yellow solution. The solid residue was extracted with an additional 40 mL of dichloromethane-methanol (1:1 v/v), and the filtrates combined. The solution was evaporated to dryness, redissolved in dichloromethane (40 mL) and the product precipitated by addition of petroleum spirits (40 mL). The solid was filtered, washed with petroleum spirits (10 mL) and dried under vacuum to give 2 as an orange solid (192 mg, 69%). Found: C 50.2; H 3.45; N 9.1. C18H15N3O3Pd requires C 50.5; H 3.5; N 9.8%. (0043) 1H NMR, delta 9.12-6.91 (m, bipy and Ph), 4.26 (s, CH2). ESI MS (added NaHCO2, capillary exit voltage 140 V): [M+Na]+ m/z 461.88 (100%), calculated for C19H15N3O3PdNa m/z 462.00.

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Reference£º
Article; Sim, Sophie A.; Saunders, Graham C.; Lane, Joseph R.; Henderson, William; Inorganica Chimica Acta; vol. 450; (2016); p. 285 – 292;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

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

[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).

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
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

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

[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).

According to the analysis of related databases, (2,2¡ä-Bipyridine)dichloropalladium(II), the application of this compound in the production field has become more and more popular.

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

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

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.

The chemical industry reduces the impact on the environment during synthesis, 52522-40-4,Tris(dibenzylideneacetone)dipalladium-chloroform,I believe this compound will play a more active role in future production and life.

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

As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 52522-40-4,Tris(dibenzylideneacetone)dipalladium-chloroform, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.52522-40-4

General procedure: 0.0813 g (0.4637mmol) of TMQ, 0.1671 g (1.159 mmol) of dmfu and 0.2000 g (0.1932 mmol) of [Pd2(DBA)3. CHCl3] were dissolved under inert atmosphere (Ar) in 30 ml of anhydrous acetone. The mixture was stirred for 60 m and eventually treated with active charcoal for 5/10 min and filtered on celite filter. The resulting yellow solution was dried under vacuum and the residual treated with diethyl ether, filtered, washed with diethyl ether in excess and dried under vacuum. 0.1104 g (yield 67percent) of the title compound was obtained as pale yellow microcrystals.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, Tris(dibenzylideneacetone)dipalladium-chloroform.

Reference£º
Article; Canovese; Visentin; Biz; Scattolin; Santo; Bertolasi; Journal of Organometallic Chemistry; vol. 786; (2015); p. 21 – 30;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

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.

Solid [Pd(bpy)Cl2] (0.166 g, 0.5 mmol) was added to dl-H2pa (0.064 g, 0.5 mmol) in ethanol (8 mL) containing triethyl amine (0.05 g, 0.5 mmol). The mixture was stirred for 72 h. The yellow-beige precipitate was filtered off, washed with ethanol and air-dried. Yield: 45%. Anal. Calcd. for C16ClH22N3O4Pd: C, 41.6; H, 4.8; N, 9.1; Cl, 7.7; Pd, 23.0%, Found: C, 41.5; H, 4.4; N, 9.0; Cl, 7.6; Pd, 23.1%. Conductivity data (10-3 M in DMF):LambdaM = 97.0 ohm-1. IR (cm-1): nu(NH) 3106; nuas(COO-) 1659; nus(COO-) 1411; nu(Pd-O) 521; nu(Pd-N) 471 cm-1. Raman: nuas(COO-) 1598; nus(COO-) 1402; delta(NH) 1560; nu(Pd-O) 529; nu(Pd-N) 450 cm-1; 1H NMR (d6-DMSO/TMS, ppm), 3.73 (d, H, Halpha); 2.50 (m, 2H, Hbeta); 2.07 (m, 2H, Hgamma); 1.30 (m, 2H, Hdelta); 3.45, 3.10 (m, 2H, Hepsilon); 13.19 (s, H, NH), ESI-MS: m/z, 816.7 {Pd(Hpa)(bpy)]2Cl}+, 780.7 {[Pd(bpy)(Hpa)]2}+, 390.0 [Pd(bpy)(Hpa)]+, 263.0 [Pd(bpy)]+.

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; Alie El-Deen, Afaf A.; El-Askalany, Abd El-Monem E.; Halaoui, Ruba; Jean-Claude, Bertrand J.; Butler, Ian S.; Mostafa, Sahar I.; Journal of Molecular Structure; vol. 1036; (2013); p. 161 – 167;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

887919-35-9,Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials.887919-35-9,A new synthetic method of this compound is introduced below.

887919-35-9, Step 14-6, Preparation of tert-butyl N-{3-[(4-{4-[2-cyano-4-(trifluoromethyl)phenyl]piperazin-1-yl}-2′-ethoxy-[1,1′-biphenyl]-3-yl)formamido]propyl}carbamate To a mixture of tert-butyl N-{3-[(5-bromo-2-{4-[2-cyano-4-(trifluoromethyl)phenyl]piperazin-1-yl}phenyl)formamido]propyl}carbamate (20.0 mg, 0.0328 mmol), 2-ethoxyphenylboronic acid (10.9 mg, 0.0657 mmol), Pd[t-Bu2P(4-NMe2C6H4)]2Cl2) (9.2 mg, 0.013 mmol), and K2CO3 (27.2 mg, 0.197 mmol) in a sealed tube was added dioxane (2 mL) and H2O (0.2 mL). The resulting mixture was degassed with N2 for 10 min and stirred at 100 C. for 30 min. The mixture was concentrated and purified by C18 reversed phase column chromatography to give the title compound (18.5 mg, 87% yield) as a white solid. LCMS (M+H)+=652.5.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, Bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II).

Reference£º
Patent; Crinetics Pharmaceuticals, Inc.; HAN, Sangdon; ZHU, Yunfei; KIM, Sun Hee; ZHAO, Jian; WANG, Shimiao; (146 pag.)US2019/367481; (2019); A1;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

Adding a certain compound to certain chemical reactions, such as: 14871-92-2,(2,2¡ä-Bipyridine)dichloropalladium(II), can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 14871-92-2,14871-92-2

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

According to the analysis of related databases, 14871-92-2, the application of this compound in the production field has become more and more popular.

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

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials.14221-01-3,A new synthetic method of this compound is introduced below.14221-01-3

Into a 20 mL brown Schlenk tube were placed Pd(PPh3)4(0.05 mmol, 0.0578 g), PdCl2(MeCN)2 (0.05 mmol, 0.0130 g), norbornene(2.1 mmol, 0.2 g), and K2CO3 (2.0 mmol, 0.277 g). Then, 4-iodotoluene (2.0 mmol, 0.26 mL) as well as 8 mL DMA (containing 0.5 M H2O) were transferred to the tube by syringe under N2. The mixturewas stirred at 70 C for 20 h. The solutionwas washed withH2O and ether. The organic layer was extracted twice with ether. It was then purified by Centrifugal Thin Layer Chromatography (CTLC)using CH2Cl2 as eluent. The solvent was removed under reduced pressure. The yield of 5a is 98% (0.0848 g, 0.0980 mmol). The residue was subjected to crystallization process by CH2Cl2 and hexanesand yellow crystals were resulted. Similar processes were taken forthe preparation of 5b except that dicyclopentadiene (2.0 mmol,0.264 g) was used. The yield of 5b is 98% (0.0922 g, 0.0980 mmol). Yellow crystals were resulted in crystallization process by CH2Cl2and heptane.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, Tetrakis(triphenylphosphine)palladium.

Reference£º
Article; Chen, Ya-Qian; Hong, Fung-E.; Tetrahedron; vol. 71; 38; (2015); p. 7016 – 7025;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

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 887919-35-9,Bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II), as follows.887919-35-9

Step 14-6, Preparation of tert-butyl N-{3-[(4-{4-[2-cyano-4-(trifluoromethyl)phenyl]piperazin-1-yl}-2′-ethoxy-[1,1′-biphenyl]-3-yl)formamido]propyl}carbamate To a mixture of tert-butyl N-{3-[(5-bromo-2-{4-[2-cyano-4-(trifluoromethyl)phenyl]piperazin-1-yl}phenyl)formamido]propyl}carbamate (20.0 mg, 0.0328 mmol), 2-ethoxyphenylboronic acid (10.9 mg, 0.0657 mmol), Pd[t-Bu2P(4-NMe2C6H4)]2Cl2) (9.2 mg, 0.013 mmol), and K2CO3 (27.2 mg, 0.197 mmol) in a sealed tube was added dioxane (2 mL) and H2O (0.2 mL). The resulting mixture was degassed with N2 for 10 min and stirred at 100 C. for 30 min. The mixture was concentrated and purified by C18 reversed phase column chromatography to give the title compound (18.5 mg, 87% yield) as a white solid. LCMS (M+H)+=652.5.

According to the analysis of related databases, Bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II), the application of this compound in the production field has become more and more popular.

Reference£º
Patent; Crinetics Pharmaceuticals, Inc.; HAN, Sangdon; ZHU, Yunfei; KIM, Sun Hee; ZHAO, Jian; WANG, Shimiao; (146 pag.)US2019/367481; (2019); A1;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method