October 13, 2020 | Catalyst palladium

The important role of (2,2¡ä-Bipyridine)dichloropalladium(II)

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.

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

To a vigorously stirred solution of BzpheH2 (32.32 mg,0.12 mmol) in 8 mL CH3OH/H2O (V:V D 1:1), [Pd(bipy)Cl2] (20 mg, 0.06 mmol) was added. The mixture was heatedto 50C and adjusted to pH D 8-9 by NaOH solution, andthen stirred for 2 h. The solution was concentrated to about80% of the original volume. The complex I-a was separatedfrom the solution after a few days. Yellow crystalline, yield: 68%. IR (KBr, cm1): n(Amide&)1551, n(OCO)a 1632, n(OCO)a1383, n(Pd-N) 566, n(Pd-O) 465. 1H NMR (600 MHz, d6-DMSO) d (ppm): 3.08 (dd, J D 13.1, 4.5 Hz, 1H, CH2-H),3.29 (dd, J D 13.1, 4.5 Hz, 1H, CH2-H), 5.08-5.05 (m, 1H,CH), 6.65 (t, J D 7.5 Hz, 1H, Ar-H), 6.73 (t, J D 7.5 Hz, 2H,Ar-H), 7.09 (d, J D 3.0 Hz, 3H, Ar-H), 7.13 (d, J D 5.4 Hz,1H, Ar-H), 7.23 (d, J D 7.2 Hz, 2H, Ar-H), 7.28 (d, J D5.4 Hz, 1H, Ar-H), 7.78-7.75 (m, 1H, Ar-H), 8.02 (t, J D7.8 Hz, 1H, Ar-H), 8.26 (d, J D 7.8 Hz, 1H, Ar-H), 8.30 (t, JD 6.9 Hz, 4H, Ar-H), 8.42 (d, J D 7.8 Hz, 1H, Ar-H). ESIMS:568.03 [MCK]C. Anal. Calcd. for [Pd(bipy)(Bzphe-N,O)] (C26H21N3O3Pd, 529.06): C, 58.93; H, 3.99; N, 7.93.Found: C, 58.84; H, 4.04; N, 7.84.

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

The origin of a common compound about Tetrakis(triphenylphosphine)palladium

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Tetrakis(triphenylphosphine)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.”14221-01-3

Into a 20 mL brown Schlenk tube were placed Pd(PPh3)4(0.05 mmol, 0.0578 g), PdCl2(MeCN)2 (0.05 mmol, 0.0130 g), norbornene(2.1 mmol, 0.2 g), and K2CO3 (2.0 mmol, 0.277 g). Then, 4-iodotoluene (2.0 mmol, 0.26 mL) as well as 8 mL DMA (containing 0.5 M H2O) were transferred to the tube by syringe under N2. The mixturewas stirred at 70 C for 20 h. The solutionwas washed withH2O and ether. The organic layer was extracted twice with ether. It was then purified by Centrifugal Thin Layer Chromatography (CTLC)using CH2Cl2 as eluent. The solvent was removed under reduced pressure. The yield of 5a is 98% (0.0848 g, 0.0980 mmol). The residue was subjected to crystallization process by CH2Cl2 and hexanesand yellow crystals were resulted. Similar processes were taken forthe preparation of 5b except that dicyclopentadiene (2.0 mmol,0.264 g) was used. The yield of 5b is 98% (0.0922 g, 0.0980 mmol). Yellow crystals were resulted in crystallization process by CH2Cl2and heptane.

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Reference£º
Article; Chen, Ya-Qian; Hong, Fung-E.; Tetrahedron; vol. 71; 38; (2015); p. 7016 – 7025;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

Downstream synthetic route of (2,2¡ä-Bipyridine)dichloropalladium(II)

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.

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

Some scientific research about Bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II)

As the rapid development of chemical substances, we look forward to future research findings about 887919-35-9

887919-35-9, Bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)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.

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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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

Brief introduction of (2,2¡ä-Bipyridine)dichloropalladium(II)

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.

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

Introduction of a new synthetic route about (2,2¡ä-Bipyridine)dichloropalladium(II)

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.

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).

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

Extracurricular laboratory: Synthetic route of (2,2¡ä-Bipyridine)dichloropalladium(II)

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

(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

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).

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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

Extracurricular laboratory: Synthetic route of Bis(tri-tert-butylphosphine)palladium

As the rapid development of chemical substances, we look forward to future research findings about 53199-31-8

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.

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.

As the rapid development of chemical substances, we look forward to future research findings about 53199-31-8

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

Application of (2,2¡ä-Bipyridine)dichloropalladium(II)

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Solid [Pd(bpy)Cl2] (0.085 g, 0.25 mmol) was added to Hdahmp(0.04 g, 0.25 mmol) in ethanol (10 mL). Et3N (0.02 cm3, 0.20 mmol)was then added and the reaction mixture was refluxed for 48 h. Abrown precipitate was obtained which was filtered off, washedwith methanol and air-dried. Yield: 81%. Anal. Calc. for C14H13ClN6-OPdS: C, 36.9; Cl, 7.8; H, 2.9; N, 18.5; S, 7.0; Pd, 23.4. Found: C,37.1; Cl, 7.8; H, 2.8; N, 18.6; S, 7.2; Pd, 23.3%. Conductivity data(103 M in DMF): KM = 88.0 ohm1 cm2 mol1.

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Reference£º
Article; El-Morsy, Fatema A.; Jean-Claude, Bertrand J.; Butler, Ian S.; El-Sayed, Shadia A.; Mostafa, Sahar I.; Inorganica Chimica Acta; vol. 423; PB; (2014); p. 144 – 155;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

Some tips on (2,2¡ä-Bipyridine)dichloropalladium(II)

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.