Catalyst palladium

The origin of a common compound about 52522-40-4

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.

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

Stage 2: Stage 1 material (8.50 g) and 3,5-bis(4-tert-butylphenyl)phenyl-1-boronic acid pinacol ester (15.50 g) were dissolved in toluene (230 mL). The solution was purged with nitrogen for 1 h before 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (66 mg) and tris(dibenzylidene)dipalladium (75 mg) were added using 10 mL of nitrogen-purged toluene. A 20wtpercent solution of tetraethylammonium hydroxide in water (60 mL) was added in one portion and the mixture as stirred for 20 h with the heating bath set to 105 ¡ãC. T.L.C. analysis indicated all the stage material had been consumed and only one fluorescent spot was observed. The reaction mixture was cooled and filtered into a separating funnel. The layers were separated and the aqueous layer extracted with toluene. The organic extracts were washed with water, dried with magnesium sulphate, filtered and concentrated to yield the crude product as a yellow/orange solid. Pure compound was obtained by column chromatography eluting with a gradient of ethyl acetate in hexanes followed by precipitation from DCM/methanol. HPLC indicated a purity of 99.75percent and a yield of 80percent (11.32g). 1H NMR (referenced to CDCl3): 7.83 (3H, d), 7.76 (6H, s), 7.73 (3H, s) 7.63 (12H, d) 7.49 (12H, d), 7.21 (3H, dd), 6.88 (3H, d), 4.28 (9H, s), 2.25 (3H, m), 1.98 (3H, m), 1.4-1.5 (57H, m), 1.23 (3H, m), 0.74 (9H, t)

Reference£º
Patent; Cambridge Display Technology Limited; Sumitomo Chemical Co., Ltd; Kamtekar, Kiran; Steudel, Annette; EP2738195; (2014); A1;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

New downstream synthetic route of 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.

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.

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

Some scientific research about 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.

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 new synthetic route of Tris(dibenzylideneacetone)dipalladium-chloroform

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).

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

Some scientific research about (2,2¡ä-Bipyridine)dichloropalladium(II)

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.

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?).

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 new synthetic route of Tris(dibenzylideneacetone)dipalladium-chloroform

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.

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 new synthetic route of (2,2¡ä-Bipyridine)dichloropalladium(II)

To a yellow suspension containing 0.10 g (0.31 mmol) of [Pd(bpy)Cl2] in water (10 mL) wereadded a solution containing 0.04 g (0.32 mmol) of HaptHCl in water (10 mL) and an aqueoussolution of NaOH (0.25 M, 2.5 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 (5 mL) wasadded to the yellow filtrate. The mixture was stood at room temperature for 2 d, and the resultingyellow crystals of [2](NO3)2 was collected by filtration. Yield: 0.03 g (36%)., 14871-92-2

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 new synthetic route of Tris(dibenzylideneacetone)dipalladium-chloroform

The origin of a common compound about (2,2¡ä-Bipyridine)dichloropalladium(II)

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.

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 new synthetic route of Tris(dibenzylideneacetone)dipalladium-chloroform

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.

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