Catalyst palladium

53199-31-8, Bis(tri-tert-butylphosphine)palladium, 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.

Example 29 Preparation of 5-(4-{3-[3-(4-fluoro-phenyl)-5-oxo-1,5-dihydro-[1,2,4]triazol-4-yl]-propenyl}-phenyl)-furan-2-carbaldehyde (compound 44) This example describes the synthesis of common ligand mimics of the invention containing a linker group following the reaction scheme shown in . Compound numbers correspond to the numbers in the figure. The compounds 4-allyl-5-(4-fluoro-phenyl)-2,4-dihydro-[1,2,4]triazol-3-one (compound 42, 500 mg, 2.28 mmol) and 5-(4-bromo-phenyl)-furfural were mixed in dioxane (10 ml), followed by the addition of diisopropylethylamine (0.795 ml, 4.56 mmol). Bis(tri-tert-butylphosphine) palladium (56 mg, 0.109 mmol) was added to the reaction mixture, which then was stirred at a temperature of 90 C. for a period of 1 hour. Volatiles were removed in vacuo, and the residue was diluted in 0.2 N HCl solution, followed by extraction with ethyl acetate. Combined organic layers were dried over MgSO4, filtered, and concentrated in vacuo. The crude product was purified by flash chromatography (gradient 7:3 to 9:1 ethyl acetate/hexanes+0.5% MeOH) to give 5-(4-{3-[3-(4-fluoro-phenyl)-5-oxo-1,5-dihydro-[1,2,4]triazol-4-yl]-propenyl}-phenyl)-furan-2-carbaldehyde (compound 44, 375 mg, 42%). 1H NMR (300 MHz, CDCl3) delta 4.55 (d, J=4.7, 2H), 6.31 (td, J=3.2, 16.0, 1H), 6.44 (d, J=16.0, 1H), 6.84 (d, J=3.7, 1H), 7.18 (dd, J=8.5, JHF=8.5, 2H), 7.32 (d, J=3.7, 1H), 7.40 (d, J=8.3, 2H), 7.61 (dd, J=8.5, JHF=5.2, 2H), 7.76 (d, J=8.3, 2H), 9.64 (s, 1H), 10.56 (s, 1H); 13C NMR (300 MHz, CDCl3) delta 43.8, 107.9, 116.3 (d, JCF=22), 123.2, 124.4, 125.6, 127.1, 128.7, 130.3 (d, JCF=9), 132.3, 137.1, 147.0, 152.2, 155.7, 158.9, 164.1 (d, JCF=250), 206.6; MS m/s 389.96 (M+1).

With the complex challenges of chemical substances, we look forward to future research findings about Bis(tri-tert-butylphosphine)palladium,belong catalyst-palladium compound

Reference£º
Patent; Yu, Lin; Dong, Qing; Pierre, Fabrice; Chang, Edcon; Lang, Hengyuan; Qin, Yong; Fang, Yunfeng; Hansen, Mark; Pellecchia, Maurizio; US2004/9526; (2004); A1;,
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

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.

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
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

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

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). 1H NMR (CDCl3, T 298 K, ppm) d: 1.37 (s, 9H, tBu), 2.99 (s, 3H,CH3 quinoline), 5.62 (broad AB system, 4H, CH]CH), 7.51 (d, 1H,J 8.4 Hz, H3), 7.58 (dd, 1H, J 8.1, 7.3 Hz, H6), 7.93 (dd, 1H, J 8.1,1.3 Hz, H5), 8.02 (dd, 1H, J 7.3, 1.3 Hz, H7), 8.22 (d, 1H, J 8.4 Hz,H4).13C{1H} NMR (CDCl3, T 298 K, ppm) d: 29.6 (CH3, CH3 quinoline),30.9 (CH3, CMe3), 54.6 (C, CMe3), 100.5 (bs, CH, CH]CH), 123.8 (CH, C3), 125.9 (CH, C6), 128.0 (C, C10), 130.3 (C, C8), 130.6 (CH, C5),138.3 (CH, C4), 138.8 (CH, C7), 149.4 (C, C9), 165.0 (C, C2), 186.9 (C,CO), 188.4 (C, CO).1H NMR (CD2Cl2, T 193 K, ppm) d: 1.26 (s, 9H, tBu), 2.87 (s, 3H,CH3 quinoline), 4.71 (d, 1H, J 5.8 Hz, CH]CH), 4.92 (d, 1H, J 5.8 Hz,CH]CH), 6.10 (d, 1H, J 9.8 Hz, CH]CH), 6.22 (d, 1H, J 9.8 Hz,CH]CH), 7.51 (d, 1H, J 8.4 Hz, H3), 7.58 (dd, 1H, J 8.1, 7.3 Hz, H6),7.96 (dd, 1H, J 8.1, 1.3 Hz, H5), 8.01 (dd, 1H, J 7.3, 1.3 Hz, H7), 8.26(d, 1H, J 8.4 Hz, H4).13C{1H} NMR (CD2Cl2, T 193 K, ppm) d: 29.0 (CH3, eCH3 quinoline),30.3 (CH3, CMe3), 54.9 (C, CMe3), 63.5 (s, CH, CH]CH), 67.6 (s,CH, CH]CH), 124.2 (CH, C3), 126.2 (CH, C6), 127.9 (C, C10), 128.9 (C,C8), 131.1 (CH, C5), 134.5 (s, CH, CH]CH), 135.3 (s, CH, CH]CH),138.8 (CH, C4), 139.2 (CH, C7), 149.2 (C, C9), 165.0 (C, C2), 186.6 (C,CO), 188.3 (C, CO). IR (KBr pellets): -CN 1575, nCO 1613; 1636 cm1. Anal calc. for C20H21NO2PdS: C, 53.88; H, 4.75; N, 3.14. Found C,53.71; H, 4.79; N, 3.01percent.

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

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

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

First, 63.6 mg (0.2 mmol)Of compounds 111-5 and 32.2 mmol (0.6 mmol)Of methanol was added to a mixture of 30 ml of anhydrous methanol and tetrahydrofuran(Volume ratio of 1: 1)Argon protection,After stirring at room temperature for 1.5 h,Followed by the addition of 66.4 mg (0.2 mmol) of cis-dichloro-1,1′-bipyridyl palladium (II)Continue to argon protection,Stirring at 25 C for 14 h,After the reaction,The resulting solid was purified by column chromatography,Get the target product,Weight 93.8 mg, yield: 85%.

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
Patent; Changchun Institute of Applied Chemistry, Chinese Academy of Sciences; Wang, Zhiyuan; Liu, Bo; Qiao, Wenqiang; (34 pag.)CN103483391; (2016); B;,
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

10 mL ofa solution of AgNO3 (0.204 g, 1.2 mmol) was added to aqueous suspension of Pd(bipy)Cl2 (0.2 g, 0.6 mmol) acidified to pH 2-3. The formed suspension was homogenized and incubated during 1 h at 60C.

As the rapid development of chemical substances, we look forward to future research findings about 14871-92-2

Reference£º
Article; Nikandrov; Grigor’Eva; Eremin; Ruzanov; Gurzhii; Belyaev; Russian Journal of General Chemistry; vol. 85; 8; (2015); p. 1992 – 1993; Zh. Obshch. Khim.; vol. 85; 8; (2015); p. 1405 – 1406,2;,
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

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.

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

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

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.14871-92-2

To a yellow suspension containing 0.20 g (0.60 mmol) of [Pd(bpy)Cl2] in water (20 mL)was added 0.08 g (0.60 mmol) of HaptHCl. After the mixture was stirred at 50 C for 7 h, theresulting yellow solution was filtered. To the yellow filtrate was added an aqueous solution ofNaClO4 (2 M, 10 mL), followed by standing at room temperature for 1 d. The resulting yellowcrystals of [1](ClO4)4 suitable for X-ray analysis were collected by filtration. Yield: 0.32 g (87%).

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

Dichloro(1,5-cyclooctadiene)palladium(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.”12107-56-1

To a 500 mL reaction was added 10 g (1,5-cyclooctadiene) palladium dichloride, the reaction flask was replaced with a nitrogen atmosphere,19.6 g of di-tert-butyl-4-dimethylaminophenylphosphine prepared in Example 1 and 200 mL of anhydrous tetrahydrofuran were added, and the mixture was stirred at room temperature for 16 hours,There is a solid precipitation,Filtration and drying gave a pale yellow powder product bis (di-tert-butyl-4-dimethylaminophenylphosphine) palladium chloride 24. 1 g,The yield was 97% (yield based on (1,5-cyclooctadiene) palladium dichloride)The purity of the product was 99.8% by XY-1A intelligent element analyzer.

With the synthetic route has been constantly updated, we look forward to future research findings about Dichloro(1,5-cyclooctadiene)palladium(II),belong catalyst-palladium compound

Reference£º
Patent; Panjin Ge Linkaimo Technology Co., Ltd.; Rao Zhihua; Gong Ningrui; (9 pag.)CN105237568; (2017); B;,
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.

As the rapid development of chemical substances, 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 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

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.

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
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