Month: September 2020

[1,1′-Bis(diphenylphosphino)ferrocene]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.”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.

With the complex challenges of chemical substances, we look forward to future research findings about [1,1′-Bis(diphenylphosphino)ferrocene]dichloropalladium(II)

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

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

[(bpy)PdCl2] (0.332 g, 1 mmol) and Tl+L (0.475 g, 1 mmol) in 10 mL of dichloromethane were stirred for 18 h at room temperature. The resulting solution was filtered and evaporated to about 1 mL in volume. Then hexane (10 mL) was added to precipitate as a red-orange solid. The solid was repeatedly washed with diethyl ether (3 ¡Á 10 mL) and dried under vacuum to give the pure complex (0.297 g, 52.31% yield, and 1 mmol). Anal. Calc. (%) for C23H16ClN5O2PdS (568.9752): C, 48.61; H, 2.84; N, 12.32; Found (%): C, 48.59; H, 2.82; N, 12.29. TOF-MS: 532.0060 [M – Cl] +. FT-IR: 2152 (m, NCN) cm-1. 1H NMR (DMSO-d6): delta 7.16-7.20 (m, 2H, H-Ar), 7.49-7.51 (m, 2H, H-Ar), 7.65 (t, 1H, H-5, 3J 7.2), 7.74 (t, 1H, H-5′, 3J 7.2), 7.91-7.99 (m, 4H, H-Ar), 8.34-8.40 (m, 4H, H-Ar), 8.76 (d, 1H, H-6, 3J 7.2), 9.09 (d, 1H, H-6′, 3J 7.2). 13C NMR (DMSO-d6): delta 114.0 (NCN), 119.9, 121.9, 124.0, 125.9, 128.9, 133.1, 137.8, 143.0, 147.0, 149.0, 150.7, 157.9.

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; Tabrizi, Leila; Zouchoune, Bachir; Zaiter, Abdallah; Inorganica Chimica Acta; vol. 499; (2020);,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

Tris(dibenzylideneacetone)dipalladium-chloroform, 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.”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)]+.

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

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, (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

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.

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.

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

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.52522-40-4, Tris(dibenzylideneacetone)dipalladium-chloroform it is a common compound, a new synthetic route is introduced below.52522-40-4

A mixture of 38 mg (0.37 mmol) Pd2(dba)3CHCl3, 100 mg (0.74mmol) of [Mo3S4Cl3(dbbpy)3]Cl and 56 mg (0.74 mmol) of thioureain 20 ml of dichloromethane was refluxed for 5 hours. An excess ofhexane was layered onto the resulting brown solution to givegreenish-brown crystals of 2. Yield: 80 mg (71percent). Anal. Calcd forC55H76N8Cl4Mo3S5Pd: C 42.7, H 5.0, N 7.2, S 10.4. Found: C 42.8,H 5.1, N 7.0, S 10.4. 1H NMR (500.13 MHz, CDCl3): delta = 9.74 (d, J =6.11 Hz, 3H), 9.03 (d, J = 5.95 Hz, 3H), 8.49 (d, J = 1.22 Hz, 3H);8.39 (d, J = 1.22 Hz, 3H); 7.58 (p, J = 4.65, J = 1.75 Hz, 6H), 6.37 (s,4H), 1.46 (s, 27H) 1.41 (s, 27H) ppm. IR (KBr, cm1): 3397 (w,sh), 3156 (m), 3127 (m), 2962 (vs), 2907 (s), 2870 (s), 1615 (vs),1545 (m), 1481 (m), 1464 (m), 1410 (s), 1367 (m), 1310 (w),1294 (w), 1255 (m), 1203 (w), 1157 (w), 1127 (w), 1079 (w),1024 (m), 901 (m), 883 (w), 852 (w), 836 (m), 744 (w), 719 (w),605 (w), 551 (w), 485 (w), 427 (w). ESI-MS (+; CH2Cl2/CH3CN):m/z = 1611 [Mo3S4(Pdtu)Cl3(dbbpy)]+, 1436 [Mo3S4(Pd)Cl3(dbbpy)]+,1327 [Mo3S4Cl3(dbbpy)]+.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand Tris(dibenzylideneacetone)dipalladium-chloroform reaction routes.

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

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.

General procedure: [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.

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

(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

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.

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

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

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.52522-40-4, Tris(dibenzylideneacetone)dipalladium-chloroform it is a common compound, a new synthetic route is introduced below.52522-40-4

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.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand Tris(dibenzylideneacetone)dipalladium-chloroform reaction routes.

Reference£º
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

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.52522-40-4, Tris(dibenzylideneacetone)dipalladium-chloroform it is a common compound, a new synthetic route is introduced below.52522-40-4

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).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand Tris(dibenzylideneacetone)dipalladium-chloroform reaction routes.

Reference£º
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

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

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.

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