Month: August 2020

As a common heterocyclic compound, it belongs to quinuclidine compound,Quinuclidine-4-carboxylic acid hydrochloride,40117-63-3,Molecular formula: C8H14ClNO125,mainly used in chemical industry, its synthesis route is as follows.

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),belong catalyst-palladium compound

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

(2,2¡ä-Bipyridine)dichloropalladium(II), cas is 14871-92-2, it is a common heterocyclic compound, the catalyst-palladium compound, its synthesis route is as follows.

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

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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

Tris(dibenzylideneacetone)dipalladium-chloroform, cas is 52522-40-4, it is a common heterocyclic compound, the catalyst-palladium compound, its synthesis route is as follows.

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

Tetrakis(triphenylphosphine)palladium, cas is 14221-01-3, it is a common heterocyclic compound, the catalyst-palladium compound, its synthesis route is as follows.

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.

As the rapid development of chemical substances, we look forward to future research findings about 14221-01-3

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

(2,2¡ä-Bipyridine)dichloropalladium(II), cas is 14871-92-2, it is a common heterocyclic compound, the catalyst-palladium compound, its synthesis route is as follows.

The new bimetallic dinuclear complex, [{PdCl(bipy)}{l-(NH2(CH2)6H2N)}{PtCl(bipy)}]Cl(ClO4), was synthesized by modificationof the procedure reported in the literature [25]. The complex[PtCl2(bipy)] (100.0 mg, 0.236 mmol) was dissolved in DMF(10 cm3) and a solution of AgClO4 (49.1 mg, 0.236 mmol) in DMF(5 cm3) was added. The mixture was stirred overnight in the dark,at room temperature. The precipitate AgCl was removed by filtrationand the resulting pale yellow solution of [PtCl(bipy)(DMF)]ClO4 was kept in a refrigerator to cool down. A suspension of[PdCl2(bipy)] complex (73.5 mg, 0.220 mmol) in 10 cm3 of DMFwas heated with stirring at 303-313 K for about 30 min. After that,the solution of 1,6-diaminohexane (25.5 mg, 0.220 mmol) in 5 cm3DMF was added dropwise. The mixture was stirred at room temperaturefor 5 h in the dark. The filtrate [PtCl(bipy)(DMF)]ClO4was added to the resulting mixture. The clear yellow solutionwas stirred for 3 h at 323 K and then for 24 h at room temperature.The solution was then evaporated and the residue washed withether. A light yellow powder was obtained and left to dry in theair. Yield (63.8 mg, 62%). Anal. Calc. for PtPdCl4O4N6C26H32(FW = 935.88): C, 33.37; H, 3.45; N, 8.98. Found: C, 33.07; H,3.80; N, 8.73%. 1H NMR characterization (D2O, 200 MHz). 1H NMR(d, ppm): 1.35-1.50 (m, CH2 C3, C4), 1.60-1.80 (m, CH2 C2, C5),2.95-3.06 (m, CH2 C1, C6), 7.30-7.42 (d, CH H5/H50(1)), 7.45-7.60 (d, CH H5/H50(2)), 7.65-7.84 (m, CH H4/H40(1)), 8.05-8.15(m CH H4/H40(2)), 8.17-8.28 m, CH H3/H30(1)), 8.32-8.40 (m, CHH3/H30(2)), 8.42-8.48 (d CH H6/H60(1)), 8.50-8.58 (d CH H6/H60(2)). IR (KBr, 4000-300 cm1): 3438 (N-H stretch); 2853, 2927(CH2 stretch); 1610 (CN stretch); 1089 (perchlorate counterion); 765, 812 (N-H wagging) (Fig. S1).

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

Reference£º
Article; Jovanovi?, Sne?ana; Petrovi?, Biljana; Petkovi?, Marijana; Bugar?i?, ?ivadin D.; Polyhedron; vol. 101; (2015); p. 206 – 214;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

(2,2¡ä-Bipyridine)dichloropalladium(II), cas is 14871-92-2, it is a common heterocyclic compound, the catalyst-palladium compound, its synthesis route is as follows.

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.

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

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, cas is 52522-40-4, it is a common heterocyclic compound, the catalyst-palladium compound, its synthesis route is as follows.

0.1328 g (0.4057 mmol) of 8-diphenylphosphine-2-methylquinoline, 0.0674 g (0.4261 mmol) of naphthoquinone and 0.2003 g(0.1935 mmol) of [Pd2(DBA)3CHCl3] were dissolved under inert atmosphere (Ar) in 30 ml of anhydrous acetone in a 100 ml necked flask. The mixture was stirred for 60 min at RT, the resulting orange solution treated with activated charcoal, filtered on a celite filter and concentrated under vacuum. The title complexwas precipitated as a paleorange solid by slow addition of diethylether, filtered off on a gooch, and washed with diethylether and n-pentane. 0.2039g (yield 89percent) of complex 1’b was obtained. 1H-NMR (300 MHz, CDCl3, T = 298 K, ppm) delta: 3.12 (s, 3H, quinoline-CH3), 4.98-5.05 (m, 2H, CH=CH) 7.06e7.13 (m, 2H, aryl naphthoquinone), 7.29-7.71 (m, 13H, H3, PPh2, aryl naphthoquinone), 7.79 (ddd,1H, J = 8.1, 7.5,1.4 Hz, H6), 7.90 (d,1H, J = 8.1, H7), 8.05 (dd, 1H, J = 7.5, 1.6 Hz, H5), 8.19 (dd, 1H, J = 8.4, 1.4 Hz, H4). 13C{1H}-NMR (CDCl3, T = 298 K, ppm) delta: 30.3 (CH3, quinoline-CH3), 62.7 (CH, CH=CH trans-N), 66.3 (d, CH, JCP = 21 Hz, CH=CH transP), 123.9 (CH, C3), 125.1 (CH, C5), 131.1 (CH, C7), 137.8 (CH, C6), 138.4 (CH, C4), 165.7 (d, C, JCP = 22.1 Hz, C9),165.7 (C, C2),184.0 (d, C, JCP = 6.2 Hz, CO transP), 185.2 (C, CO transN). 31P{1H}-NMR (CD2Cl2, T = 298 K, ppm) delta: 23.4. IR (KBr, pellet, cm-1): 1641 (nCO). Anal. Calcd. for C32H24NO2PPd: C 64.93, H 4.09, N 2.37. Found: C 65.06, H 3.98, N 2.21.

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

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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

As a common heterocyclic compound, it belong catalyst-palladium compound,Dichloro(1,5-cyclooctadiene)palladium(II),12107-56-1,Molecular formula: C8H12Cl2Pd,mainly used in chemical industry, its synthesis route is as follows.

To a 500 mL reaction was added 10 g (1,5-cyclooctadiene) palladium dichloride, the reaction flask was replaced with a nitrogen atmosphere,19.6 g of di-tert-butyl-4-dimethylaminophenylphosphine prepared in Example 1 and 200 mL of anhydrous tetrahydrofuran were added, and the mixture was stirred at room temperature for 16 hours,There is a solid precipitation,Filtration and drying gave a pale yellow powder product bis (di-tert-butyl-4-dimethylaminophenylphosphine) palladium chloride 24. 1 g,The yield was 97% (yield based on (1,5-cyclooctadiene) palladium dichloride)The purity of the product was 99.8% by XY-1A intelligent element analyzer.

With the synthetic route has been constantly updated, we look forward to future research findings about Dichloro(1,5-cyclooctadiene)palladium(II),belong catalyst-palladium compound

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Patent; Panjin Ge Linkaimo Technology Co., Ltd.; Rao Zhihua; Gong Ningrui; (9 pag.)CN105237568; (2017); B;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

(2,2¡ä-Bipyridine)dichloropalladium(II), cas is 14871-92-2, it is a common heterocyclic compound, the catalyst-palladium compound, its synthesis route is as follows.

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%).

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

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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

Tris(dibenzylideneacetone)dipalladium-chloroform, cas is 52522-40-4, it is a common heterocyclic compound, the catalyst-palladium compound, its synthesis route is as follows.

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).

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

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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