Day: October 21, 2020

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

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).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. 52522-40-4, We look forward to the emergence of more reaction modes in the future.

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,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

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

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

72287-26-4,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. [1,1′-Bis(diphenylphosphino)ferrocene]dichloropalladium(II),72287-26-4, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of Example 246A (48 mg, 0.11 mmol) and Example 246B (25 mg, 0.11 mmol) in EtOH (1 mL) and toluene (1 mL) under an argon atmosphere were added 2M Na2CO3 (0.165 mL, 0.33 mmol) followed by Pd(PPh3)4 (13 mg, 0.011 mmol)). The resulting suspension was stirred under argon at 85¡ã C. for 2 hours. The reaction was cooled to ambient temperature, concentrated and purified by preparative HPLC to give the title compound (8.8 mg). HPLC Rt=2.203 min. m/z=446.08., 72287-26-4

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, 72287-26-4.

Reference£º
Patent; Fink, Brian E.; Gavai, Ashvinikumar V.; Vite, Gregory D.; Han, Wen-Ching; Misra, Raj N.; Xiao, Hai-Yun; Norris, Derek J.; Tokarski, John S.; US2005/250753; (2005); A1;,
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 72287-26-4,[1,1′-Bis(diphenylphosphino)ferrocene]dichloropalladium(II), as follows.72287-26-4

To a solution of Example 246A (48 mg, 0.11 mmol) and Example 246B (25 mg, 0.11 mmol) in EtOH (1 mL) and toluene (1 mL) under an argon atmosphere were added 2M Na2CO3 (0.165 mL, 0.33 mmol) followed by Pd(PPh3)4 (13 mg, 0.011 mmol)). The resulting suspension was stirred under argon at 85¡ã C. for 2 hours. The reaction was cooled to ambient temperature, concentrated and purified by preparative HPLC to give the title compound (8.8 mg). HPLC Rt=2.203 min. m/z=446.08.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. 72287-26-4, We look forward to the emergence of more reaction modes in the future.

Reference£º
Patent; Fink, Brian E.; Gavai, Ashvinikumar V.; Vite, Gregory D.; Han, Wen-Ching; Misra, Raj N.; Xiao, Hai-Yun; Norris, Derek J.; Tokarski, John S.; US2005/250753; (2005); A1;,
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.

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.

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; 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 14871-92-2,(2,2¡ä-Bipyridine)dichloropalladium(II), as follows.14871-92-2

[Pd(bpy)Cl2] (0.10 g, 0.30 mmol) was suspended in water (4 mL). Lactic acid (0.03 g, 0.28 mmol) and 1 M NaOH (0.60 mL) were dissolved in water (10 mL) and then added to the mixture, which was heated under reflux at 150 C with continuous stirring until a clear yellow solution was obtained. The solution was filtered and acetone (10 mL) was added to the solution. The reaction mixture was cooled to 4 C for a long time (2 months), resulting yellow crystals of complex 5. Yield: 33%. m.p.: 250 C. Elemental Anal. Calc. for C13H13ClN2OPd (355.10): C, 44.0; H, 3.7; N, 7.9. Found: C, 44.1; H, 3.6; N, 7.8%. IR (KBr, numax/cm-1): 1634 s, nu(CO); 1621 s, nu(CC); 1496 m, 1443 s, nu(CC,CN). Far-IR (Nujol, numax/cm-1): 333 m, nu(Pd-Cl); 285 m, nu(Pd-C); 243 m, nu(Pd-N). 1H NMR (CDCl3, delta/ppm): 2.40 (s, 3H, c), 3.01 (s, 2H, a), 7.61 (m, 2H, 5,5?), 8.02 (m, 4H, 3,3? and 4,4?), 9.31, 9.51 (2d, 2H, 6,6?).

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; 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

14871-92-2,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.14871-92-2,A new synthetic method of this compound is introduced below.

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.

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

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

52522-40-4, 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, A mixture of 38 mg (0.37 mmol) Pd2(dba)3CHCl3, 100 mg (0.74mmol) of [Mo3S4Cl3(dbbpy)3]Cl and 56 mg (0.74 mmol) of thioureain 20 ml of dichloromethane was refluxed for 5 hours. An excess ofhexane was layered onto the resulting brown solution to givegreenish-brown crystals of 2. Yield: 80 mg (71percent). Anal. Calcd forC55H76N8Cl4Mo3S5Pd: C 42.7, H 5.0, N 7.2, S 10.4. Found: C 42.8,H 5.1, N 7.0, S 10.4. 1H NMR (500.13 MHz, CDCl3): delta = 9.74 (d, J =6.11 Hz, 3H), 9.03 (d, J = 5.95 Hz, 3H), 8.49 (d, J = 1.22 Hz, 3H);8.39 (d, J = 1.22 Hz, 3H); 7.58 (p, J = 4.65, J = 1.75 Hz, 6H), 6.37 (s,4H), 1.46 (s, 27H) 1.41 (s, 27H) ppm. IR (KBr, cm1): 3397 (w,sh), 3156 (m), 3127 (m), 2962 (vs), 2907 (s), 2870 (s), 1615 (vs),1545 (m), 1481 (m), 1464 (m), 1410 (s), 1367 (m), 1310 (w),1294 (w), 1255 (m), 1203 (w), 1157 (w), 1127 (w), 1079 (w),1024 (m), 901 (m), 883 (w), 852 (w), 836 (m), 744 (w), 719 (w),605 (w), 551 (w), 485 (w), 427 (w). ESI-MS (+; CH2Cl2/CH3CN):m/z = 1611 [Mo3S4(Pdtu)Cl3(dbbpy)]+, 1436 [Mo3S4(Pd)Cl3(dbbpy)]+,1327 [Mo3S4Cl3(dbbpy)]+.

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; Laricheva, Yuliya A.; Gushchin, Artem L.; Abramov, Pavel A.; Sokolov, Maxim N.; Polyhedron; vol. 154; (2018); p. 202 – 208;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method