Day: September 14, 2020

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.

Mefenamic acid (0.40 mmol) was dissolved in methanol (15 mL) followed by the addition of KOH (0.40 mmol). After 60 min of stirring, the resulting solution was slowly added to an aqueous solution of [PdCl2(bipy)] (0.20 mmol). After 40 min of constant stirring, the yellow solid obtained was collected by filtration, washed with ethanol and dried in a desiccator with P4O10. The yield was 63%. Anal. Calc. for [Pd(C15H14NO2)2(bipy)] (%): C 64.6; H 4.88;N 7.54. Found: C 63.3; H 4.74; N 7.62. The complex is soluble inchloroform and insoluble in water and DMSO. As already observed for the Pd-tra complex, no single crystals were obtained to perform an X ray structural characterization. The [PdCl2(bipy)] complexused as a precursor in the synthesis of Pd-mef was synthesized as described in the literature [21].

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; Carvalho, Marcos A.; Arruda, Eduardo G.R.; Profirio, Daniel M.; Gomes, Alexandre F.; Gozzo, Fabio C.; Formiga, Andre L.B.; Corbi, Pedro P.; Journal of Molecular Structure; vol. 1100; (2015); p. 6 – 13;,
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., 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; 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

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.

(bpy)PdCl2 (167 mg, 0.5 mmol) and AgNO3 (170 mg, 1.0 mmol) was mixed in CH3NO2 (40 mL). The mixture was stirred at 60 C for 24 hrs, and the white AgCl precipitate was filtered by a short pad of celite. The filtrate was sampled for ESI-HRMS, and cationic C20H18N4O2Pd22+ (m/z: 279.9743) was observed. Then the filtrate was concentrated and recrystallized to give 25 mg light yellow needle-like solid. Yield 9.0%.

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; Yang, Zhenyu; Ni, Yuxin; Liu, Rui; Song, Kaixuan; Lin, Shaohui; Pan, Qinmin; Tetrahedron Letters; vol. 58; 21; (2017); p. 2034 – 2037;,
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

52522-40-4, A mixture of 55 mg (0.53 mmol) Pd2(dba)3CHCl3 and 200 mg(0.11 mmol) of [Mo3S4Cl3(dnbpy)3]PF6 in 20 ml of dichloromethanewas refluxed for 1 day. An excess of hexane was layeredonto the resulting brown solution to give brown crystals of 3.Yield: 113 mg (57percent). Anal. Calcd for C84H132N6Cl4Mo3S4Pd: C53.4, H 7.0, N 4.5, S 6.8. Found: C 53.6, H 7.1, N 4.4, S 6.9. 1HNMR (500.13 MHz, CDCl3): delta = 9.78 (d, J = 5.75 Hz, 3H), 9.35 (d, J= 5.62 Hz, 3H), 7.99 (s, 3H); 7.93 (s, 3H); 7.25 (d, J = 5.50, 6H),2.76 (t, J = 6.75 Hz, 6H), 2.71 (t, J = 7.7 Hz, 6H), 1.68 (p, J12 = 7.95,J23 = 7.82 Hz, 6H), 1.39 (p, J12 = 7.7, J23 = 7.1 Hz, 6H), 1.29 (s, 72H),0.89 (s, 18H) ppm. IR (KBr, cm1): 3376 (w, sh), 3223 (w), 3123(w), 2923 (s), 2852 (s), 1648 (w), 1614 (vs), 1554 (m), 1486 (m),1462 (m), 1415 (s), 1376 (w), 1338 (w), 1314 (w), 1260 (m),1188 (w), 1096 (s), 1021 (m), 913 (w), 873 (m), 802 (m),766 (w), 721 (w), 698 (w), 615 (w), 474 (w), 421 (w). ESI-MS(+; CH2Cl2/CH3CN): m/z = 1893 {H[Mo3S4(PdCl)Cl3(dnbpy)]}+,1855 [Mo3S4(Pd)Cl3(dnbpy)]+, 1348 [Mo3S4Cl3(dnbpy)]+.

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; Laricheva, Yuliya A.; Gushchin, Artem L.; Abramov, Pavel A.; Sokolov, Maxim N.; Polyhedron; vol. 154; (2018); p. 202 – 208;,
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

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] (0.20 g, 0.60 mmol) was suspended in water (25 mL). Silver nitrate (0.20 g, 1.19 mmol) in water (5 mL) was added and the reaction mixture was stirred for 6 h at 60 C and then at room temperature, always in absence of light. The resulting solution was centrifuged and filtered to remove AgCl. A few drops of water, glycolic acid (0.05 g, 0.66 mmol) and 1 M NaOH (1.20 mL) were added to the filtrate. The resulting solution was stirred for 5 days and concentrated at 60 C to 5 mL on a rotary evaporator. The mixture was cooled to room temperature and the yellow powder was filtered off and dissolved from water and again concentrated to 5 mL. Yellow single crystals suitable for X-ray diffraction were obtained from the resulting solution by slow evaporation at room temperature. Yield: 41%, m.p.: 212 C. Elemental Anal. Calc. for C12H16N2O6Pd (390.67): C, 36.9; H, 4.1; N, 7.2. Found: C, 36.7; H, 4.0; N, 7.1%. MS (FAB+): m/z [assignment(relative intensity)]: 337(35) [M+], 262(94), 157(100). IR (KBr, numax/cm-1): 3376 m,br, 3207 m,br, nu(OH); 1626 s, nu(CC), nuasym(CO2); 1497 w, 1451 m, nu(CC,CN); 1370 m, nusim(CO2); 415 m. Far-IR (Nujol, numax/cm-1): 385 s, nu(Pd-O); 252 m, nu(Pd-N). 1H NMR (CD3OD, delta/ppm): 4.35 (s, 2H, b), 7.71 (m, 2H, 5,5?), 8.28 (m, 2H, 4,4?), 8.39 (d, 2H, 3,3?), 8.49 (d, 2H, 6,6?). 13C NMR (CD3OD, delta/ppm): 72.71 (1C, b), 124.93 (2C, 3,3?), 128.64, 129.04 (2C, 5,5?), 142.44, 142.78 (2C, 4,4?), 150.10, 151.44 (2C, 6,6?). UV-Vis (numax/cm-1): 36101, 30120, 26525 (Reflectance).

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; 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, 72287-26-4,[1,1′-Bis(diphenylphosphino)ferrocene]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. 72287-26-4

To a solution of Example 246A (48 mg, 0.11 mmol) and Example 246B (25 mg, 0.11 mmol) in EtOH (1 mL) and toluene (1 mL) under an argon atmosphere were added 2M Na2CO3 (0.165 mL, 0.33 mmol) followed by Pd(PPh3)4 (13 mg, 0.011 mmol)). The resulting suspension was stirred under argon at 85¡ã C. for 2 hours. The reaction was cooled to ambient temperature, concentrated and purified by preparative HPLC to give the title compound (8.8 mg). HPLC Rt=2.203 min. m/z=446.08.

This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,72287-26-4,[1,1′-Bis(diphenylphosphino)ferrocene]dichloropalladium(II),its application will become more common.

Reference£º
Patent; Fink, Brian E.; Gavai, Ashvinikumar V.; Vite, Gregory D.; Han, Wen-Ching; Misra, Raj N.; Xiao, Hai-Yun; Norris, Derek J.; Tokarski, John S.; US2005/250753; (2005); A1;,
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

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%.

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
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

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 stirred suspension of [Pd(bpy)Cl2] (0.03 g, 0.1 mmol) or[Pd(phen)Cl2] (0.04 g, 0.1 mmol) in MeOH (10 mL) a solution ofHhmbt (0.023 g, 0.1 mmol) in MeOH containing KOH (0.006 g,0.1 mmol; 10 mL) was added drop by drop with stirring. The reactionmixture was warmed for 48 h, upon which a yellow-orangeprecipitate was filtered off, washed with MeOH, Et2O and driedin vacuo.For[Pd(bpy)(hmbt)]Cl2H2O: Yield: 0.07 g (51%). ElementalAnal.: Calcd. C, 49.5; H, 4.3; N, 12.6; Pd, 19.1 (C23H24N5O3Pd);Found: C, 49.7; H, 4.2; N, 12.7; Pd, 19.1%. Conductivity data(103 M in DMF): KM = 84.0 ohm1. IR (cm1): m(CN), 1621;m(CO), 1251; m(N-N), 1141; m(Pd-O), 500; m(Pd-N), 459. Raman(cm1): m(CN), 1602; m(CO), 1251; m(N-N), 1141; m(Pd-O), 501;m(Pd-N), 460. 1H NMR (ppm): 8.00 (H(3), d, J = 6 Hz, 1H); 7.75(H(6), S, 1H); 7.86 (H(7), d, J = 5.4 Hz, 1H); 7.73 (H(8), t, J = 5 Hz,1H); 7.69 (H(9), t, J = 5 Hz, 1H); 7.22 (H(10), d, J = 5.2 Hz, 1H);2.50 (CH3, S, 3H). MS (m/z): 486.4 (Calcd. 486.4), 368.2 (Calcd.368.4), 292.4 (Calcd. 292.4), 262.4 (Calcd. 262.4), 156.3 (Calcd.156.0).For[Pd(phen)(hmbt)]ClH2O: Yield: 0.08 g (54%). ElementalAnal.: Calcd. C, 53.2; H, 3.9; N, 12.4; Pd, 18.7 (C25H22N5O2Pd);Found: C, 53.3; H, 4.0; N, 12.3; Pd, 18.6%. Conductivity data(103 M in DMF): KM = 81.0 ohm1. IR (cm1): m(CN), 1600;m(CO), 1252; m(N-N), 1138; m(Pd-O), 564; m(Pd-N), 495. Raman(cm1): m(CN), 1604; m(CO), 1252; m(N-N), 1139; m(Pd-O), 565;m(Pd-N), 495. 1H NMR (ppm): 7.96 (H(3), d, J = 5.1 Hz, 1H); 7.30(H(6), S, 1H); 7.60 (H(7), d, J = 4.5 Hz, 1H); 7.77 (H(8), t,J = 4.2 Hz, 1H); 7.73 (H(9), t, J = 4.5 Hz, 1H); 7.22 (H(10), d,J = 4.2 Hz, 1H); 2.50 (CH3, S, 3H). MS (m/z): 510.4 (Calcd. 510.4),286.4 (Calcd. 286.4), 180.6 (Calcd. 180.0).

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; El-Asmy, Hala A.; Butler, Ian S.; Mouhri, Zhor S.; Jean-Claude, Bertrand J.; Emmam, Mohamed S.; Mostafa, Sahar I.; Journal of Molecular Structure; vol. 1059; 1; (2014); p. 193 – 201;,
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.

(bpy)PdCl2 (167 mg, 0.5 mmol) and AgNO3 (170 mg, 1.0 mmol) was mixed in CH3NO2 (40 mL). The mixture was stirred at 60 C for 24 hrs, and the white AgCl precipitate was filtered by a short pad of celite. The filtrate was sampled for ESI-HRMS, and cationic C20H18N4O2Pd22+ (m/z: 279.9743) was observed. Then the filtrate was concentrated and recrystallized to give 25 mg light yellow needle-like solid. Yield 9.0%.

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; Yang, Zhenyu; Ni, Yuxin; Liu, Rui; Song, Kaixuan; Lin, Shaohui; Pan, Qinmin; Tetrahedron Letters; vol. 58; 21; (2017); p. 2034 – 2037;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method