Day: September 2, 2020

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

To 50.0 mg (0.0483 mmol, 1 equiv.) of Pd2dba3?CHCl3 in 1.5mL of anhydrous acetone was added 134.0 mg (1.449 mmol, 30 equiv.) of norbornadiene and 27.0 mg(0.242 mmol, 5 equiv.) of N-methylmaleimide under an atmosphere of argon. The reaction mixture wasstirred for 30 min at room temperature, upon which noticeable palladium black had accumulated in thereaction vessel. The reaction mixture was transferred via cannula and filtered under argon to provide atranslucent yellow-green solution. The solution was briefly concentrated in vacuo to provide a moreviscous, yellow-green oil, to which 5.0 mL of anhydrous Et2O was added. This provided an opaque,yellow-green suspension of Pd(NBD)(NMM) catalyst as a fine yellow powder, which was usedimmediately in the coupling reaction, to avoid degradation.

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; Nytko, Frederick E.; Shukla, Krupa H.; DeShong, Philip; Heterocycles; vol. 8; 2; (2014); p. 1465 – 1476;,
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.

A suspension of 1 mmol (0.333 g) of [Pd(bpy)Cl2] in 150 mL ofacetone was treated with 1 mmol (0.228 g) of benzyl dithiocarbamatesodium salt and the mixture was refluxed under continuousmagnetic stirring for 2 h. Stirring continued for another 12 h at 318 K and then filtered.The resulting yellow colored filtrate containing the desired productwas concentrated to 15 mL at 318 K. The orange precipitate formedwas filtered off and washed with diethyl ether. Recrystallizationwas done by dissolving the precipitate in minimum amount ofethanol. Yield: 0.336 g (70%) and decomposes at 207-209 C. Anal.Calcd. for C18H16N3S2ClPd (480.34 g mol-1) Found, (Calcd.) (%): C45.01, (45.05); H, 3.36 (3.34); N, 8.75 (8.76). Molar conductance forthe complex (10-3 M, H2O) is 9.0 mS m2 mol-1. FT-IR (KBr, cm-1):3405 upsilon(N-H); 3020 upsilon(Caro-H); 1550 upsilon(C-N); 1313 upsilons (CNS); 1036 upsilonas(CNS); 503 upsilon (Pd-N); 450 upsilon (Pd-S). 1H NMR (DMSO-d6-D2O, delta ppm):4.71 (d, 2H, H-c), 7.40 (m,1H, H-a), 7.32 (m, 4H, H-b), 8.54 (m, 2H, H-6,60), 8.27 (m, 2H, H-3,30), 8.18 (m, 2H, H-4,40), 7.68 (M, 2H, H-5,50)(Fig. 1). 13C NMR (DMSO-d6, delta ppm): 48.00 (C-e), 139.67 (C-5,5′),139.84 (C-4,4′), 140.00 (C-a), 140.17 (C-b), 140.34 (C-c), 140.50 (C-3,30), 140.60 (C-d), 140.67 (C-1,10), 140.76 (C-f) (Fig. 1). The NMRnumbering schemes are given in Fig. 1. UV-Vis data (H2O, lambdamax/nm,(log epsilon)): 312 (3.40), 249 (3.75), 187 (3.94).

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; Saeidifar, Maryam; Mirzaei, Hamidreza; Ahmadi Nasab, Navid; Mansouri-Torshizi, Hassan; Journal of Molecular Structure; vol. 1148; (2017); p. 339 – 346;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

A common heterocyclic compound, 14221-01-3,Tetrakis(triphenylphosphine)palladium, 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. 14221-01-3

Into a 20 mL brown Schlenk tube were placed Pd(PPh3)4(0.05 mmol, 0.0578 g), PdCl2(MeCN)2 (0.05 mmol, 0.0130 g), norbornene(2.1 mmol, 0.2 g), and K2CO3 (2.0 mmol, 0.277 g). Then, 4-iodotoluene (2.0 mmol, 0.26 mL) as well as 8 mL DMA (containing 0.5 M H2O) were transferred to the tube by syringe under N2. The mixturewas stirred at 70 C for 20 h. The solutionwas washed withH2O and ether. The organic layer was extracted twice with ether. It was then purified by Centrifugal Thin Layer Chromatography (CTLC)using CH2Cl2 as eluent. The solvent was removed under reduced pressure. The yield of 5a is 98% (0.0848 g, 0.0980 mmol). The residue was subjected to crystallization process by CH2Cl2 and hexanesand yellow crystals were resulted. Similar processes were taken forthe preparation of 5b except that dicyclopentadiene (2.0 mmol,0.264 g) was used. The yield of 5b is 98% (0.0922 g, 0.0980 mmol). Yellow crystals were resulted in crystallization process by CH2Cl2and heptane.

This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,Tetrakis(triphenylphosphine)palladium,14221-01-3,its application will become more common.

Reference£º
Article; Chen, Ya-Qian; Hong, Fung-E.; Tetrahedron; vol. 71; 38; (2015); p. 7016 – 7025;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

10025-98-6 A common heterocyclic compound, 10025-98-6,Potassium chloropalladite, 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.

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.

This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,Potassium chloropalladite,10025-98-6,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

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

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.

This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,Tris(dibenzylideneacetone)dipalladium-chloroform,52522-40-4,its application will become more common.

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

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

c) N1-[2-phenyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-phenyl]-1-benzenesulfonamide. A mixture of the N1-(4-bromo-2-phenylbenzene)-1-benzenesulfonamide (0.388 g, 1.00 mmol), bis(pinacolato)diboron (0.305 g, 1.20 mmol), potassium acetate (0.294 g, 3.00 mmol) and [1,1′-bis(diphenylphosphino) ferrocene]dichloropalladium(II) (25 mg, 0.030 mmol) in DMF (10 ml) was heated under an atmosphere of nitrogen at 100¡ã C. for 16.5 hours. The DMF was evaporated in vacuo and the residue purified by silica gel flash chromatography using methylene chloride/heptane 7:3 plus 2percent triethyl amine to provide N1-[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-2-phenylbenzene]-1-benzenesulfonamide (0.135 g) as an oil. tR=23.13 min (RP-HPLC, 25-100percent acetonitrile-0.1percent TFA, 25 min); low resolution MS m/e 434 (M-H+)

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

Reference£º
Patent; CALDERWOOD, DAVID; ARNOLD, LEE; MAZDIYASNI, HORMOZ; HIRST, GAVIN C.; DENG, BOJUAN B.; JOHNSTON, DAVID N.; RAFFERTY, PAUL; TOMETZKI, GERALD B.; TWIGGER, HELEN L.; MUNSCHAUER, RAINER; US2003/187001; (2003); A1;,
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.

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

A common heterocyclic compound, 887919-35-9,Bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)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. 887919-35-9

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.

This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,887919-35-9,Bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II),its application will become more common.

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

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.

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%)., 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.

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

Name is (2,2¡ä-Bipyridine)dichloropalladium(II), as a common heterocyclic compound, it belongs to catalyst-palladium compound, and cas is 14871-92-2, its synthesis route is as follows.,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)]+.

With the complex challenges of chemical substances, we look forward to future research findings about (2,2¡ä-Bipyridine)dichloropalladium(II)

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