Category: catalyst-palladium

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

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

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

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

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

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

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.

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, 14871-92-2.

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

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

Direct synthesis from 1a, CF3SO3Ag, and [Pd(bipy)Cl2]. A solution of Pd(bipy)Cl2 (0.10 g, 0.30 mmol) in 5 mL of CH3CN and a solution of CF3SO3Ag (0.15 g, 0.58 mmol) in 5 mL of CH3CN were mixed and heated under reflux for a day. Precipitates were filtered off and the solvent was evaporated. The resultant pale yellow powder was dissolved in a mixture of CH3CN and CHCl3, and then 1a (0.35 g, 0.58 mmol) was added. The mixture was heated under reflux for a day, and then, filtered and the solvents were removed under reduced pressure. Resultant material was recrystallized from CH3CN- CHCl3 mixture twice. White fibers (0.27 g, 46.0%) were obtained. Mp. 249-252 C (dec.). 1H NMR ( CDCl3/CD3CN = 4/1, v/v, 300 MHz): delta 10.41 (brs, 8H, OH), 9.35 (brs, 4H, Py-H), 8.33 (d, J = 7.5 Hz, 2H, bipy-H), 8.26 (t, J = 7.0 Hz, 2H, bipy-H), 7.92 (brs, 4H, Py-H), 7.51 (t, 2H, bipy-H), 7.26 (d, J = 4.4 Hz, 2H, bipy- H), 6.99 (s, 4H, ArH), 6.95 (s, 4H, ArH), 6.89 (s, 4H, ArH), 6.67 (s, 4H, ArH), 4.11 (d, J = 13.8 Hz, 2H. CH2), 4.02 (d, J = 13.6 Hz, 4H. CH2), 3.80 (brs, 4H, CH2), 3.66 (brd, J = 10.8 Hz, 4H, CH2), 3.47 (brd, J = 13.8 Hz, 4H. CH2), 3.43 (brd, J = 12.9 Hz, 2H. CH2), 3.32 (d, J = 12.9 Hz, 4H, CH2), 2.19, 2.17 (s, 24H, CH3). 13C NMR ( CDCl3/CD3CN = 4/1, v/v, 75.6 MHz): delta 157.0, 153.2, 151.7, 150.7, 149.7, 147.2, 142.3, 131.2, 131.1, 130.0, 129.6, 129.5, 128.2, 128.0, 127.8, 127.8, 127.7, 124.2, 123.0, 121.0, 118.8, 57.7, 56.7, 32.0, 31.5, 20.5, 20.3. FABMS: m/z: 1611.5 ( M+); HRMS (FAB): calcd for C89H88F3N6O11S106Pd ( M2+ + TflO-), 1611.5219. Found: 1611.5231.

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; Takemura, Hiroyuki; Mogami, Yukako; Okayama, Kanae; Nagashima, Noriko; Orioka, Kana; Hayano, Yuri; Kobayashi, Asako; Iwanaga, Tetsuo; Sako, Katsuya; Journal of Inclusion Phenomena and Macrocyclic Chemistry; vol. 95; 3-4; (2019); p. 235 – 246;,
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.

General procedure: Silver tetrafluoroborate (AgBF4) (0.6 mmol) was dissolvedin methanol (7 mL); (2,2?-bipyridine) dichloropalladium(II)(Pd(Bpy)Cl2) (0.3 mmol) was dissolved in DMSO (1 mL),and then, the solutions were stirred together at ambient temperature0.5 h. Following gravity filtration, solid 3-hydroxyflavonederivative (0.3 mmol) and triethylamine (0.7 mL)were added to the filtrate. The reaction mixture was stirredfor 0.5 h (2 h for the Fla-OMe). The corresponding bipyridinepalladium flavonolato salt was then recovered usingvacuum filtration and recrystallized in CH3OH/CH3CN solvent;remaining solvent was removed in a vacuum desiccatorovernight.[(PdII(Bpy)(3-Hydroxy-4?-methoxyFla)][BF4] complex1 Yield: 129 mg, 70% (orange crystals) Found: C, 50.51;H, 3.01; N, 4.52; Calcd for C26H19BF4N2O4Pd:C, 50.64;H, 3.11; N, 4.54. UV-Vis lambdamax (CH3CN/nm)(epsilon/M-1 cm-1) (444 (25 200); 1H NMR (CD3CN, 400 MHz): delta 7.92 (d,J = 6.5 Hz, 2H), 7.85 (m, J = 21.9 Hz, 4H), 7.65 (t, J = 18.7,2H), 7.47 (d, J = 7.3 Hz, 2H), 7.28 (t, J = 11.4 Hz, 1 H),7.19 (d, J = 6.5 Hz, 2 H), 7.13 (t, J = 13.9 Hz, 1 H), 6.66 (d,J = 8.1 Hz, 2 H); 13C NMR (CD3CN, 400 MHz): delta = 181.44,161.13, 153.96, 153.65, 152.62, 151.82, 150.65, 148.54,148.20, 140.94, 140.67, 138.01, 133.05, 129.37, 129.14,127.34, 127.27, 125.04, 124.44, 124.03, 123.10, 123.01,121.96, 121.73, 117.45, 115.53, 54.91 ppm. ESI MS: m/z(pos.) 529.04., 14871-92-2

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; Han, Xiaozhen; Whitfield, Sarah; Cotten, Jacob; Transition Metal Chemistry; (2019);,
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(2,2?-bpy)Cl2 (67 mg, 0.2 mmol) was stirred with AgNO3 (68 mg, 0.4 mmol) in water (10 mL) with light excluded at 40 C for 12 h. The suspension obtained was cooled to 0 C in ice bath for 30 min. Then AgCl was removed from the solution by filtration. 1 (52.8 mg, 0.2 mmol) was added to the clear filtrate and pH was measured and found to be 2.0. Then the mixture was stirred at 40 C for 2 h. The resulting light yellow solution was concentrated to a volume of 5 mL at 40 C on a rotary evaporator. Yellow cubes were obtained after one day. The yield was 85 mg (60%). 1H NMR (D2O, pD 2.0, 298 K, delta, ppm): 1?, 3.69 (12 H, s, CH3), 3.60 (4H, s, CH2), 7.93 (4H, s, H6); 2,2?-bpy, 7.23 (4H, dd, H5, 3JH-H = 6.0 Hz, 4JH-H = 3.0 Hz), 7.60 (4H, t, H5?, 3JH-H = 7.2 Hz), 7.79 (4H, dd, H6, 3JH-H = 6.0 Hz), 7.94-8.18 (20H, m, H3,H3?,H4,H4?,H6?).

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; Khutia, Anupam; Shen, Wei-Zheng; Das, Neeladri; Sanz Miguel, Pablo J.; Lippert, Bernhard; Inorganica Chimica Acta; vol. 417; (2014); p. 274 – 286;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method