Tag: M.W:300-400

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: 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., 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; 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

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: 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.

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; 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

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

To a yellow suspension containing 0.30 g (0.90 mmol) of [Pd(bpy)Cl2] in water (20 mL) wereadded a solution containing 0.06 g (0.46 mmol) of HaptHCl in water (10 mL) and an aqueoussolution of NaOH (0.3 M, 10 mL). When the mixture was stirred at 50 C for 3 h, the suspensionturned to a yellow solution. After filtration, a saturated aqueous solution of NaNO3 (10 mL) wasadded to the yellow filtrate, followed by storing in a refrigerator for 1 week. The resulting yellowcrystals of [3](NO3)2 suitable for X-ray analysis were collected by filtration. Yield: 0.19 g (55%).

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; 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

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: 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 desiccator overnight., 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; 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 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.

Synthesis of [Pd{OC(O)CH2N(COPh)}(bipy)] 2 A mixture of [PdCl2(bipy)] (210 mg, 0.63 mmol) with hippuric acid (113 mg, 0.63 mmol) and silver(I) oxide (600 mg) in dichloromethane (30 mL) was refluxed for 3.5 h. Methanol (30 mL) was added, and the mixture filtered to give a clear yellow solution. The solid residue was extracted with an additional 40 mL of dichloromethane-methanol (1:1 v/v), and the filtrates combined. The solution was evaporated to dryness, redissolved in dichloromethane (40 mL) and the product precipitated by addition of petroleum spirits (40 mL). The solid was filtered, washed with petroleum spirits (10 mL) and dried under vacuum to give 2 as an orange solid (192 mg, 69%). Found: C 50.2; H 3.45; N 9.1. C18H15N3O3Pd requires C 50.5; H 3.5; N 9.8%. (0043) 1H NMR, delta 9.12-6.91 (m, bipy and Ph), 4.26 (s, CH2). ESI MS (added NaHCO2, capillary exit voltage 140 V): [M+Na]+ m/z 461.88 (100%), calculated for C19H15N3O3PdNa m/z 462.00.

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; Sim, Sophie A.; Saunders, Graham C.; Lane, Joseph R.; Henderson, William; Inorganica Chimica Acta; vol. 450; (2016); p. 285 – 292;,
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

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.

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; 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, 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

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.

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; 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

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,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

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