Month: August 2020

(2,2¡ä-Bipyridine)dichloropalladium(II), cas is 14871-92-2, it is a common heterocyclic compound, the catalyst-palladium compound, its synthesis route is as follows.

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.

With the rapid development of chemical substances, we look forward to future research findings about (2,2¡ä-Bipyridine)dichloropalladium(II)

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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

Tris(dibenzylideneacetone)dipalladium-chloroform, cas is 52522-40-4, it is a common heterocyclic compound, the catalyst-palladium compound, its synthesis route is as follows.

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).

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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

(2,2¡ä-Bipyridine)dichloropalladium(II), cas is 14871-92-2, it is a common heterocyclic compound, the catalyst-palladium compound, its synthesis route is as follows.

A suspension of 1 mmol (0.333 g) of [Pd(bpy)Cl2] in 150 mL ofacetone was treated with 1 mmol (0.228 g) of benzyl dithiocarbamatesodium salt and the mixture was refluxed under continuousmagnetic stirring for 2 h. Stirring continued for another 12 h at 318 K and then filtered.The resulting yellow colored filtrate containing the desired productwas concentrated to 15 mL at 318 K. The orange precipitate formedwas filtered off and washed with diethyl ether. Recrystallizationwas done by dissolving the precipitate in minimum amount ofethanol. Yield: 0.336 g (70%) and decomposes at 207-209 C. Anal.Calcd. for C18H16N3S2ClPd (480.34 g mol-1) Found, (Calcd.) (%): C45.01, (45.05); H, 3.36 (3.34); N, 8.75 (8.76). Molar conductance forthe complex (10-3 M, H2O) is 9.0 mS m2 mol-1. FT-IR (KBr, cm-1):3405 upsilon(N-H); 3020 upsilon(Caro-H); 1550 upsilon(C-N); 1313 upsilons (CNS); 1036 upsilonas(CNS); 503 upsilon (Pd-N); 450 upsilon (Pd-S). 1H NMR (DMSO-d6-D2O, delta ppm):4.71 (d, 2H, H-c), 7.40 (m,1H, H-a), 7.32 (m, 4H, H-b), 8.54 (m, 2H, H-6,60), 8.27 (m, 2H, H-3,30), 8.18 (m, 2H, H-4,40), 7.68 (M, 2H, H-5,50)(Fig. 1). 13C NMR (DMSO-d6, delta ppm): 48.00 (C-e), 139.67 (C-5,5′),139.84 (C-4,4′), 140.00 (C-a), 140.17 (C-b), 140.34 (C-c), 140.50 (C-3,30), 140.60 (C-d), 140.67 (C-1,10), 140.76 (C-f) (Fig. 1). The NMRnumbering schemes are given in Fig. 1. UV-Vis data (H2O, lambdamax/nm,(log epsilon)): 312 (3.40), 249 (3.75), 187 (3.94).

With the rapid development of chemical substances, we look forward to future research findings about (2,2¡ä-Bipyridine)dichloropalladium(II)

Reference£º
Article; Saeidifar, Maryam; Mirzaei, Hamidreza; Ahmadi Nasab, Navid; Mansouri-Torshizi, Hassan; Journal of Molecular Structure; vol. 1148; (2017); p. 339 – 346;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

Bis(tri-tert-butylphosphine)palladium, cas is 53199-31-8, it is a common heterocyclic compound, the catalyst-palladium compound, its synthesis route is as follows.

B. Synthesis of 3-(1-pyrrolidinyl)phenol 7g (30 mmol) of 1-Bromo-3-methoxymethoxy-benzene from step A and 2,5 g (35 mmol) of pyrrolidine were dissolved under argon in 60 mL of toluene. Then, 0.15 g (0.3 mmol) of bis(tri-t-butylphosphine)palladium(0), 2,5g KOH und 0,6g (0,15 mmol) cetyltrimethylammoniumbromid were added, and the reaction mixture was heated at 80 C. At the end of the reaction, the reaction mixture was poured into 200 mL of ethyl acetate, and the organic phase was extracted with 1 N sodium hydroxide solution and then dried with magnesium sulfate. The solvent was distilled off in a rotary evaporator, and the residue was purified on silica gel using heptane/ethyl acetate (8/0,8). The product thus obtained was dissolved in 15 mL of ethanol and mixed with 10 mL of a 2.9 molar solution of ethanolic hydrochloric acid.

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Patent; Wella Aktiengesellschaft; EP1752192; (2007); A1;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

Potassium chloropalladite, cas is 10025-98-6, it is a common heterocyclic compound, the catalyst-palladium compound, its synthesis route is as follows.

General procedure: 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.

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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

Bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II), cas is 887919-35-9, it is a common heterocyclic compound, the catalyst-palladium compound, its synthesis route is as follows.

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.

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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

A common heterocyclic compound, the catalyst-palladium compound, name is (2,2¡ä-Bipyridine)dichloropalladium(II),cas is 14871-92-2, mainly used in chemical industry, its synthesis route is as follows.

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.

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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

A common heterocyclic compound, the catalyst-palladium compound, name is Tris(dibenzylideneacetone)dipalladium-chloroform,cas is 52522-40-4, mainly used in chemical industry, its synthesis route is as follows.

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.

As the rapid development of chemical substances, we look forward to future research findings about 52522-40-4

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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

A common heterocyclic compound, the catalyst-palladium compound, name is Tris(dibenzylideneacetone)dipalladium-chloroform,cas is 52522-40-4, mainly used in chemical industry, its synthesis route is as follows.

0.1624 g (0.4076 mmol) of 1,2-bis(diphenylphosphine)ethane, 0.1671 g (1.159 mmol) of dmfu and 0.2002 g (0.1934 mmol) of [Pd2(DBA)3*CHCl3] were dissolved under inert atmosphere (Ar) in 30 ml of anhydrous acetone and vigorously stirred for 60 min. Owing to the progressive dissolution of [Pd2(DBA)3*CHCl3], the violet color of the mixture gradually disappeared and the concomitant precipitation of the scarcely soluble pale yellow complex 1j was observed. The solution was dried under vacuum, the residue dissolved in CH2Cl2, treated with activated charcoal and filtered on a celite filter. The clear pale yellow solution was concentrated under vacuum and the title complex precipitated by slow addition of diethylether. Complex 1j was filtered off on a gooch, washed with diethylether and dried under vacuum. 0.2027 g (yield 81percent) of the title complex 1j as a pale yellow solid was obtained. 1H NMR (300 MHz, CDCl3, T = 298 K, ppm) delta: 2.11-2.61 (m, 4H, CH2P), 3.40 (s, 3H, OCH3), 4.33-4.42 (m, 2H, CH=CH), 7.32-7.53 (m, 16H, PPh), 7.79-7.85 (m, 4H, PPh). 13C{1H} NMR (CDCl3, T = 298 K, ppm selected peaks) delta: 26.7 (m CH2, CH2P), 50.5 (CH3, OCH3), 52.9 (m, CH, CH=CH), 173.7 (C, CO). 31P{1H} NMR (CD2Cl2, T = 298 K, ppm) delta: 39.0. IR (KBr, pellet, cm-1): 1683 (nCO). Anal. Calcd. for C32H32O4P2Pd: C 59.22, H 4.97. Found: C 59.11, H 5.03.

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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

The catalyst-palladium compound, name is (2,2¡ä-Bipyridine)dichloropalladium(II),cas is 14871-92-2, mainly used in chemical industry, its synthesis route is as follows.

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

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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