Day: October 12, 2020

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.

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; 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

52522-40-4, 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

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

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

General procedure: 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 75%) of the title compound was obtained as pale yellow microcrystals.

The chemical industry reduces the impact on the environment during synthesis, Tris(dibenzylideneacetone)dipalladium-chloroform, , I believe this compound will play a more active role in future production and life.

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

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: 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)]+.

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; 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

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.

Direct synthesis from 1a, CF3SO3Ag, and [Pd(bipy)Cl2]. A solution of Pd(bipy)Cl2 (0.10 g, 0.30 mmol) in 5 mL of CH3CN and a solution of CF3SO3Ag (0.15 g, 0.58 mmol) in 5 mL of CH3CN were mixed and heated under reflux for a day. Precipitates were filtered off and the solvent was evaporated. The resultant pale yellow powder was dissolved in a mixture of CH3CN and CHCl3, and then 1a (0.35 g, 0.58 mmol) was added. The mixture was heated under reflux for a day, and then, filtered and the solvents were removed under reduced pressure. Resultant material was recrystallized from CH3CN- CHCl3 mixture twice. White fibers (0.27 g, 46.0%) were obtained. Mp. 249-252 C (dec.). 1H NMR ( CDCl3/CD3CN = 4/1, v/v, 300 MHz): delta 10.41 (brs, 8H, OH), 9.35 (brs, 4H, Py-H), 8.33 (d, J = 7.5 Hz, 2H, bipy-H), 8.26 (t, J = 7.0 Hz, 2H, bipy-H), 7.92 (brs, 4H, Py-H), 7.51 (t, 2H, bipy-H), 7.26 (d, J = 4.4 Hz, 2H, bipy- H), 6.99 (s, 4H, ArH), 6.95 (s, 4H, ArH), 6.89 (s, 4H, ArH), 6.67 (s, 4H, ArH), 4.11 (d, J = 13.8 Hz, 2H. CH2), 4.02 (d, J = 13.6 Hz, 4H. CH2), 3.80 (brs, 4H, CH2), 3.66 (brd, J = 10.8 Hz, 4H, CH2), 3.47 (brd, J = 13.8 Hz, 4H. CH2), 3.43 (brd, J = 12.9 Hz, 2H. CH2), 3.32 (d, J = 12.9 Hz, 4H, CH2), 2.19, 2.17 (s, 24H, CH3). 13C NMR ( CDCl3/CD3CN = 4/1, v/v, 75.6 MHz): delta 157.0, 153.2, 151.7, 150.7, 149.7, 147.2, 142.3, 131.2, 131.1, 130.0, 129.6, 129.5, 128.2, 128.0, 127.8, 127.8, 127.7, 124.2, 123.0, 121.0, 118.8, 57.7, 56.7, 32.0, 31.5, 20.5, 20.3. FABMS: m/z: 1611.5 ( M+); HRMS (FAB): calcd for C89H88F3N6O11S106Pd ( M2+ + TflO-), 1611.5219. Found: 1611.5231.

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; Takemura, Hiroyuki; Mogami, Yukako; Okayama, Kanae; Nagashima, Noriko; Orioka, Kana; Hayano, Yuri; Kobayashi, Asako; Iwanaga, Tetsuo; Sako, Katsuya; Journal of Inclusion Phenomena and Macrocyclic Chemistry; vol. 95; 3-4; (2019); p. 235 – 246;,
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

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.

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

Potassium chloropalladite, 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.”10025-98-6

General procedure: 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.

As the rapid development of chemical substances, we look forward to future research findings about 10025-98-6

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

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

Under inert gas protection,Tri-tert-butylphosphonium tetrafluoroborate (9.3 g, 0.032 mil,4Eq), tris (dibenzylideneacetone) dipalladium () chloroform adduct (8. 3g, 008 mol, leq) and 200 mlDimethyl sulfoxide was added to the reaction flask,And then slowly dropping to them1M sodium methoxide solution in methanol(32L, 0.032, 0e, 4eq),50 ¡ã C for 15 h.Gloves bag filter,The filter cake was washed with dimethyl sulfoxideThe The filter cake was dried in n-hexane.filter,The filtrate was concentrated and crystallized.filter,The filter cake was washed with a small amount of n-hexane and the filter cake was washed with a small amount of n-hexane and dried to give 3. 27 g of a white solid powder in 80percent yield, elemental analysis: C, 56.17;H, 10. 50; P, 12. 07; Pd, 21.26

The chemical industry reduces the impact on the environment during synthesis, Tris(dibenzylideneacetone)dipalladium-chloroform, , I believe this compound will play a more active role in future production and life.

Reference£º
Patent; Hebei bailingwei super fine material Co. Ltd.; Wang, Zhen; Liu, YunSheng; Deng, XongFei; (5 pag.)CN105273009; (2016); A;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

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 3-4, Preparation of tert-butyl (3R)-4-[4-(2-ethoxypyridin-3-yl)-3-fluoro-2-(methoxycarbonyl)phenyl]-3-ethylpiperazine-1-carboxylate To a mixture of tert-butyl (3R)-4-[4-bromo-3-fluoro-2-(methoxycarbonyl)phenyl]-3-ethylpiperazine-1-carboxylate (267 mg, 0.600 mmol), (2-ethoxypyridin-3-yl)boronic acid (150 mg, 0.900 mmol), Pd[t-Bu2P(4-NMe2C6H4)]2Cl2) (42.5 mg, 0.0600 mmol), and K2CO3 (249 mg, 1.80 mmol) in a sealed tube was added dioxane (4 mL) and H2O (0.4 mL). The resulting solution was degassed with N2 (g) for 10 min, sealed, and stirred at 100 C. for 30 min. The reaction was treated with additional (2-ethoxypyridin-3-yl)boronic acid (37.8 mg, 0.226 mmol), Pd[t-Bu2P(4-NMe2C6H4)]2Cl2) (13.4 mg, 0.0189 mmol), and K2CO3 (78.3 mg, 0.567 mmol) and stirred at 100 C. for additional 30 min. The mixture was concentrated and purified by C18 reversed phase column chromatography to give the title compound (255 mg, 87% yield) as a brown gum. LCMS (M+H)+: 488.4.

With the synthetic route has been constantly updated, we look forward to future research findings about Bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II),belong catalyst-palladium compound

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