Category: catalyst-palladium

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.

Solid [Pd(bpy)Cl2] (0.166 g, 0.5 mmol) was added to dl-H2pa (0.064 g, 0.5 mmol) in ethanol (8 mL) containing triethyl amine (0.05 g, 0.5 mmol). The mixture was stirred for 72 h. The yellow-beige precipitate was filtered off, washed with ethanol and air-dried. Yield: 45%. Anal. Calcd. for C16ClH22N3O4Pd: C, 41.6; H, 4.8; N, 9.1; Cl, 7.7; Pd, 23.0%, Found: C, 41.5; H, 4.4; N, 9.0; Cl, 7.6; Pd, 23.1%. Conductivity data (10-3 M in DMF):LambdaM = 97.0 ohm-1. IR (cm-1): nu(NH) 3106; nuas(COO-) 1659; nus(COO-) 1411; nu(Pd-O) 521; nu(Pd-N) 471 cm-1. Raman: nuas(COO-) 1598; nus(COO-) 1402; delta(NH) 1560; nu(Pd-O) 529; nu(Pd-N) 450 cm-1; 1H NMR (d6-DMSO/TMS, ppm), 3.73 (d, H, Halpha); 2.50 (m, 2H, Hbeta); 2.07 (m, 2H, Hgamma); 1.30 (m, 2H, Hdelta); 3.45, 3.10 (m, 2H, Hepsilon); 13.19 (s, H, NH), ESI-MS: m/z, 816.7 {Pd(Hpa)(bpy)]2Cl}+, 780.7 {[Pd(bpy)(Hpa)]2}+, 390.0 [Pd(bpy)(Hpa)]+, 263.0 [Pd(bpy)]+., 14871-92-2

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; Alie El-Deen, Afaf A.; El-Askalany, Abd El-Monem E.; Halaoui, Ruba; Jean-Claude, Bertrand J.; Butler, Ian S.; Mostafa, Sahar I.; Journal of Molecular Structure; vol. 1036; (2013); p. 161 – 167;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

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. 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)]+.

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; 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

A common heterocyclic compound, 52522-40-4,Tris(dibenzylideneacetone)dipalladium-chloroform, 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

0.1127g (0.4871mmol) of Me-TtBQ, 0.1755g (1.218mmol) of dmfu and 0.2101g (0.2030mmol) of [Pd2(DBA)3¡¤CHCl3] were dissolved under inert atmosphere (Ar) in 30ml of anhydrous acetone. The mixture was stirred for 60min and eventually treated with active charcoal for 5/10min and filtered on Celite filter. The resulting yellow solution was dried under vacuum and the residual treated with diethyl ether, filtered off, washed with diethyl ether in excess and dried under vacuum. 0.1452g (yield 75percent) of the title compound was obtained as pale yellow microcrystals.

This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,52522-40-4,Tris(dibenzylideneacetone)dipalladium-chloroform,its application will become more common.

Reference£º
Article; Canovese, Luciano; Visentin, Fabiano; Biz, Chiara; Scattolin, Thomas; Santo, Claudio; Bertolasi, Valerio; Polyhedron; vol. 102; (2015); p. 94 – 102;,
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.

Pd(2,2?-bpy)Cl2 (67 mg, 0.2 mmol) was stirred with AgNO3 (68 mg, 0.4 mmol) in water (10 mL) with light excluded at 40 C for 12 h. The suspension obtained was cooled to 0 C in ice bath for 30 min. Then AgCl was removed from the solution by filtration. 1 (52.8 mg, 0.2 mmol) was added to the clear filtrate and pH was measured and found to be 2.0. Then the mixture was stirred at 40 C for 2 h. The resulting light yellow solution was concentrated to a volume of 5 mL at 40 C on a rotary evaporator. Yellow cubes were obtained after one day. The yield was 85 mg (60%). 1H NMR (D2O, pD 2.0, 298 K, delta, ppm): 1?, 3.69 (12 H, s, CH3), 3.60 (4H, s, CH2), 7.93 (4H, s, H6); 2,2?-bpy, 7.23 (4H, dd, H5, 3JH-H = 6.0 Hz, 4JH-H = 3.0 Hz), 7.60 (4H, t, H5?, 3JH-H = 7.2 Hz), 7.79 (4H, dd, H6, 3JH-H = 6.0 Hz), 7.94-8.18 (20H, m, H3,H3?,H4,H4?,H6?).

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; Khutia, Anupam; Shen, Wei-Zheng; Das, Neeladri; Sanz Miguel, Pablo J.; Lippert, Bernhard; Inorganica Chimica Acta; vol. 417; (2014); p. 274 – 286;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

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. 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

This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,(2,2¡ä-Bipyridine)dichloropalladium(II),14871-92-2,its application will become more common.

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

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.

Pd(2,2?-bpy)Cl2 (67 mg, 0.2 mmol) was stirred with AgNO3 (68 mg, 0.4 mmol) in water (10 mL) with light excluded at 40 C for 12 h. The suspension obtained was cooled to 0 C in ice bath for 30 min. Then AgCl was removed from the solution by filtration. 1 (52.8 mg, 0.2 mmol) was added to the clear filtrate and pH was measured and found to be 2.0. Then the mixture was stirred at 40 C for 2 h. The resulting light yellow solution was concentrated to a volume of 5 mL at 40 C on a rotary evaporator. Yellow cubes were obtained after one day. The yield was 85 mg (60%). 1H NMR (D2O, pD 2.0, 298 K, delta, ppm): 1?, 3.69 (12 H, s, CH3), 3.60 (4H, s, CH2), 7.93 (4H, s, H6); 2,2?-bpy, 7.23 (4H, dd, H5, 3JH-H = 6.0 Hz, 4JH-H = 3.0 Hz), 7.60 (4H, t, H5?, 3JH-H = 7.2 Hz), 7.79 (4H, dd, H6, 3JH-H = 6.0 Hz), 7.94-8.18 (20H, m, H3,H3?,H4,H4?,H6?).

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; Khutia, Anupam; Shen, Wei-Zheng; Das, Neeladri; Sanz Miguel, Pablo J.; Lippert, Bernhard; Inorganica Chimica Acta; vol. 417; (2014); p. 274 – 286;,
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.

[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?).

This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,(2,2¡ä-Bipyridine)dichloropalladium(II),14871-92-2,its application will become more common.

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

A common heterocyclic compound, 52522-40-4,Tris(dibenzylideneacetone)dipalladium-chloroform, 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.

This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,52522-40-4,Tris(dibenzylideneacetone)dipalladium-chloroform,its application will become more common.

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

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. 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.

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; 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

A common heterocyclic compound, 52522-40-4,Tris(dibenzylideneacetone)dipalladium-chloroform, 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

0.1127g (0.4871mmol) of Me-TtBQ, 0.1755g (1.218mmol) of dmfu and 0.2101g (0.2030mmol) of [Pd2(DBA)3¡¤CHCl3] were dissolved under inert atmosphere (Ar) in 30ml of anhydrous acetone. The mixture was stirred for 60min and eventually treated with active charcoal for 5/10min and filtered on Celite filter. The resulting yellow solution was dried under vacuum and the residual treated with diethyl ether, filtered off, washed with diethyl ether in excess and dried under vacuum. 0.1452g (yield 75percent) of the title compound was obtained as pale yellow microcrystals.

This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,52522-40-4,Tris(dibenzylideneacetone)dipalladium-chloroform,its application will become more common.

Reference£º
Article; Canovese, Luciano; Visentin, Fabiano; Biz, Chiara; Scattolin, Thomas; Santo, Claudio; Bertolasi, Valerio; Polyhedron; vol. 102; (2015); p. 94 – 102;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method