Month: November 2020

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

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).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 52522-40-4, other downstream synthetic routes, hurry up and to see.

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.

[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)., 14871-92-2

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 14871-92-2, other downstream synthetic routes, hurry up and to see.

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

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.,14871-92-2

General procedure: To a vigorously stirred solution of BzpheH2 (32.32 mg, 0.12 mmol) in 8 mL CH3OH/H2O (V:V 1:1), [Pd(bipy)Cl2] (20 mg, 0.06 mmol) was added. The mixture was heated to 50C and adjusted to pH 8-9 by NaOH solution, and then stirred for 2 h. The solution was concentrated to about 80% of the original volume. The complex I-a was separated from the solution after a few days.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 14871-92-2.

Reference£º
Article; Wang, Li-Wei; Liu, Si-Yuan; Wang, Jin-Jie; Peng, Wen; Li, Sheng-Hui; Zhou, Guo-Qiang; Qin, Xin-Ying; Wang, Shu-Xiang; Zhang, Jin-Chao; Synthesis and Reactivity in Inorganic, Metal-Organic, and Nano-Metal Chemistry; vol. 45; 7; (2015); p. 1049 – 1056;,
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.

The new bimetallic dinuclear complex, [{PdCl(bipy)}{l-(NH2(CH2)6H2N)}{PtCl(bipy)}]Cl(ClO4), was synthesized by modificationof the procedure reported in the literature [25]. The complex[PtCl2(bipy)] (100.0 mg, 0.236 mmol) was dissolved in DMF(10 cm3) and a solution of AgClO4 (49.1 mg, 0.236 mmol) in DMF(5 cm3) was added. The mixture was stirred overnight in the dark,at room temperature. The precipitate AgCl was removed by filtrationand the resulting pale yellow solution of [PtCl(bipy)(DMF)]ClO4 was kept in a refrigerator to cool down. A suspension of[PdCl2(bipy)] complex (73.5 mg, 0.220 mmol) in 10 cm3 of DMFwas heated with stirring at 303-313 K for about 30 min. After that,the solution of 1,6-diaminohexane (25.5 mg, 0.220 mmol) in 5 cm3DMF was added dropwise. The mixture was stirred at room temperaturefor 5 h in the dark. The filtrate [PtCl(bipy)(DMF)]ClO4was added to the resulting mixture. The clear yellow solutionwas stirred for 3 h at 323 K and then for 24 h at room temperature.The solution was then evaporated and the residue washed withether. A light yellow powder was obtained and left to dry in theair. Yield (63.8 mg, 62%). Anal. Calc. for PtPdCl4O4N6C26H32(FW = 935.88): C, 33.37; H, 3.45; N, 8.98. Found: C, 33.07; H,3.80; N, 8.73%. 1H NMR characterization (D2O, 200 MHz). 1H NMR(d, ppm): 1.35-1.50 (m, CH2 C3, C4), 1.60-1.80 (m, CH2 C2, C5),2.95-3.06 (m, CH2 C1, C6), 7.30-7.42 (d, CH H5/H50(1)), 7.45-7.60 (d, CH H5/H50(2)), 7.65-7.84 (m, CH H4/H40(1)), 8.05-8.15(m CH H4/H40(2)), 8.17-8.28 m, CH H3/H30(1)), 8.32-8.40 (m, CHH3/H30(2)), 8.42-8.48 (d CH H6/H60(1)), 8.50-8.58 (d CH H6/H60(2)). IR (KBr, 4000-300 cm1): 3438 (N-H stretch); 2853, 2927(CH2 stretch); 1610 (CN stretch); 1089 (perchlorate counterion); 765, 812 (N-H wagging) (Fig. S1).

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 (2,2¡ä-Bipyridine)dichloropalladium(II) reaction routes.

Reference£º
Article; Jovanovi?, Sne?ana; Petrovi?, Biljana; Petkovi?, Marijana; Bugar?i?, ?ivadin D.; Polyhedron; vol. 101; (2015); p. 206 – 214;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a downstream synthesis route of the compound 14871-92-2,14871-92-2

General procedure: Solid [Pd(L)Cl2] (L = bpy, phen) (0.2 mmol) was added to methanolic solution H2mesc (0.039 g, 0.2 mmol) containing KOH (0.0224 g, 0.4 mmol;; 15 mL). The mixture was stirred for 24 h. The yellow precipitate was filtered off, washed with methanol and air-dried. For [Pd(bpy)(mesc)]: Anal. Calc. For C20H15N2O4.5Pd: C, 52.0; H, 3.3; N, 6.1; Pd, 23.1%, Found: C, 52.1, H, 3.2; N, 6.0; Pd, 23.0%. Conductivity data (10-3 M in DMSO): LambdaM = 2.0 Ohm-1 cm2 mol-1. IR (cm-1); nu(C=O) 1664; nu(C-C) 1486; nu(C-O) 1254; nu(Pd-O) 521; nu(Pd-N) 427. 1H NMR (d6-DMSO/TMS, ppm), delta: CH3, 3.36; H(3), 6.66; H(8), 5.90; H(5), 6.50. ESI-MS: m/z: 905 (Calcd 904.8) [Pd(bpy)(mesc)]2+, 453 (Calcd 452.4) [Pd(bpy)(mesc)]+., 14871-92-2

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 14871-92-2.

Reference£º
Article; Butler, Ian S.; Gilson, Denis F.R.; Jean-Claude, Bertrand J.; Mostafa, Sahar I.; Inorganica Chimica Acta; vol. 423; PB; (2014); p. 132 – 143;,
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 52522-40-4,Tris(dibenzylideneacetone)dipalladium-chloroform, as follows.52522-40-4

52522-40-4, 0.1328 g (0.4057 mmol) of 8-diphenylphosphine-2-methylquinoline, 0.0674 g (0.4261 mmol) of naphthoquinone and 0.2003 g(0.1935 mmol) of [Pd2(DBA)3CHCl3] were dissolved under inert atmosphere (Ar) in 30 ml of anhydrous acetone in a 100 ml necked flask. The mixture was stirred for 60 min at RT, the resulting orange solution treated with activated charcoal, filtered on a celite filter and concentrated under vacuum. The title complexwas precipitated as a paleorange solid by slow addition of diethylether, filtered off on a gooch, and washed with diethylether and n-pentane. 0.2039g (yield 89percent) of complex 1’b was obtained. 1H-NMR (300 MHz, CDCl3, T = 298 K, ppm) delta: 3.12 (s, 3H, quinoline-CH3), 4.98-5.05 (m, 2H, CH=CH) 7.06e7.13 (m, 2H, aryl naphthoquinone), 7.29-7.71 (m, 13H, H3, PPh2, aryl naphthoquinone), 7.79 (ddd,1H, J = 8.1, 7.5,1.4 Hz, H6), 7.90 (d,1H, J = 8.1, H7), 8.05 (dd, 1H, J = 7.5, 1.6 Hz, H5), 8.19 (dd, 1H, J = 8.4, 1.4 Hz, H4). 13C{1H}-NMR (CDCl3, T = 298 K, ppm) delta: 30.3 (CH3, quinoline-CH3), 62.7 (CH, CH=CH trans-N), 66.3 (d, CH, JCP = 21 Hz, CH=CH transP), 123.9 (CH, C3), 125.1 (CH, C5), 131.1 (CH, C7), 137.8 (CH, C6), 138.4 (CH, C4), 165.7 (d, C, JCP = 22.1 Hz, C9),165.7 (C, C2),184.0 (d, C, JCP = 6.2 Hz, CO transP), 185.2 (C, CO transN). 31P{1H}-NMR (CD2Cl2, T = 298 K, ppm) delta: 23.4. IR (KBr, pellet, cm-1): 1641 (nCO). Anal. Calcd. for C32H24NO2PPd: C 64.93, H 4.09, N 2.37. Found: C 65.06, H 3.98, N 2.21.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 52522-40-4, and friends who are interested can also refer to it.

Reference£º
Article; Canovese, Luciano; Scattolin, Thomas; Visentin, Fabiano; Santo, Claudio; Journal of Organometallic Chemistry; vol. 834; (2017); p. 10 – 21;,
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

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

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; 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

887919-35-9 A common heterocyclic compound, 887919-35-9,Bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)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.

Step 3-4, Preparation of tert-butyl (3R)-4-[4-(2-ethoxypyridin-3-yl)-3-fluoro-2-(methoxycarbonyl)phenyl]-3-ethylpiperazine-1-carboxylate To a mixture of tert-butyl (3R)-4-[4-bromo-3-fluoro-2-(methoxycarbonyl)phenyl]-3-ethylpiperazine-1-carboxylate (267 mg, 0.600 mmol), (2-ethoxypyridin-3-yl)boronic acid (150 mg, 0.900 mmol), Pd[t-Bu2P(4-NMe2C6H4)]2Cl2) (42.5 mg, 0.0600 mmol), and K2CO3 (249 mg, 1.80 mmol) in a sealed tube was added dioxane (4 mL) and H2O (0.4 mL). The resulting solution was degassed with N2 (g) for 10 min, sealed, and stirred at 100 C. for 30 min. The reaction was treated with additional (2-ethoxypyridin-3-yl)boronic acid (37.8 mg, 0.226 mmol), Pd[t-Bu2P(4-NMe2C6H4)]2Cl2) (13.4 mg, 0.0189 mmol), and K2CO3 (78.3 mg, 0.567 mmol) and stirred at 100 C. for additional 30 min. The mixture was concentrated and purified by C18 reversed phase column chromatography to give the title compound (255 mg, 87% yield) as a brown gum. LCMS (M+H)+: 488.4.

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 Bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II) reaction routes.

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

The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. 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.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 14871-92-2.

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

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 52522-40-4,Tris(dibenzylideneacetone)dipalladium-chloroform, as follows.52522-40-4

To 50.0 mg (0.0483 mmol, 1 equiv.) of Pd2dba3?CHCl3 in 1.5mL of anhydrous acetone was added 134.0 mg (1.449 mmol, 30 equiv.) of norbornadiene and 27.0 mg(0.242 mmol, 5 equiv.) of N-methylmaleimide under an atmosphere of argon. The reaction mixture wasstirred for 30 min at room temperature, upon which noticeable palladium black had accumulated in thereaction vessel. The reaction mixture was transferred via cannula and filtered under argon to provide atranslucent yellow-green solution. The solution was briefly concentrated in vacuo to provide a moreviscous, yellow-green oil, to which 5.0 mL of anhydrous Et2O was added. This provided an opaque,yellow-green suspension of Pd(NBD)(NMM) catalyst as a fine yellow powder, which was usedimmediately in the coupling reaction, to avoid degradation.

According to the analysis of related databases, Tris(dibenzylideneacetone)dipalladium-chloroform, the application of this compound in the production field has become more and more popular.

Reference£º
Article; Nytko, Frederick E.; Shukla, Krupa H.; DeShong, Philip; Heterocycles; vol. 8; 2; (2014); p. 1465 – 1476;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method