Month: August 2020

As a common heterocyclic compound, it belongs to quinuclidine compound,Quinuclidine-4-carboxylic acid hydrochloride,40117-63-3,Molecular formula: C8H14ClNO249,mainly used in chemical industry, its synthesis route is as follows.,53199-31-8

Example 29 Preparation of 5-(4-{3-[3-(4-fluoro-phenyl)-5-oxo-1,5-dihydro-[1,2,4]triazol-4-yl]-propenyl}-phenyl)-furan-2-carbaldehyde (compound 44) This example describes the synthesis of common ligand mimics of the invention containing a linker group following the reaction scheme shown in . Compound numbers correspond to the numbers in the figure. The compounds 4-allyl-5-(4-fluoro-phenyl)-2,4-dihydro-[1,2,4]triazol-3-one (compound 42, 500 mg, 2.28 mmol) and 5-(4-bromo-phenyl)-furfural were mixed in dioxane (10 ml), followed by the addition of diisopropylethylamine (0.795 ml, 4.56 mmol). Bis(tri-tert-butylphosphine) palladium (56 mg, 0.109 mmol) was added to the reaction mixture, which then was stirred at a temperature of 90 C. for a period of 1 hour. Volatiles were removed in vacuo, and the residue was diluted in 0.2 N HCl solution, followed by extraction with ethyl acetate. Combined organic layers were dried over MgSO4, filtered, and concentrated in vacuo. The crude product was purified by flash chromatography (gradient 7:3 to 9:1 ethyl acetate/hexanes+0.5% MeOH) to give 5-(4-{3-[3-(4-fluoro-phenyl)-5-oxo-1,5-dihydro-[1,2,4]triazol-4-yl]-propenyl}-phenyl)-furan-2-carbaldehyde (compound 44, 375 mg, 42%). 1H NMR (300 MHz, CDCl3) delta 4.55 (d, J=4.7, 2H), 6.31 (td, J=3.2, 16.0, 1H), 6.44 (d, J=16.0, 1H), 6.84 (d, J=3.7, 1H), 7.18 (dd, J=8.5, JHF=8.5, 2H), 7.32 (d, J=3.7, 1H), 7.40 (d, J=8.3, 2H), 7.61 (dd, J=8.5, JHF=5.2, 2H), 7.76 (d, J=8.3, 2H), 9.64 (s, 1H), 10.56 (s, 1H); 13C NMR (300 MHz, CDCl3) delta 43.8, 107.9, 116.3 (d, JCF=22), 123.2, 124.4, 125.6, 127.1, 128.7, 130.3 (d, JCF=9), 132.3, 137.1, 147.0, 152.2, 155.7, 158.9, 164.1 (d, JCF=250), 206.6; MS m/s 389.96 (M+1).

With the complex challenges of chemical substances, we look forward to future research findings about Bis(tri-tert-butylphosphine)palladium,belong catalyst-palladium compound

Reference£º
Patent; Yu, Lin; Dong, Qing; Pierre, Fabrice; Chang, Edcon; Lang, Hengyuan; Qin, Yong; Fang, Yunfeng; Hansen, Mark; Pellecchia, Maurizio; US2004/9526; (2004); A1;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

As a common heterocyclic compound, it belongs to quinuclidine compound,Quinuclidine-4-carboxylic acid hydrochloride,40117-63-3,Molecular formula: C8H14ClNO213,mainly used in chemical industry, its synthesis route is as follows.,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)

With the complex challenges of chemical substances, we look forward to future research findings about Tris(dibenzylideneacetone)dipalladium-chloroform,belong catalyst-palladium compound

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

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

tetrakis(triphenylphosphine)palladium(0) [generated in situ from tris(diphenylmethylideneacetone)dipalladium chloroform adduct (16 mg, 0.016 mmol) and triphenylphosphine 312 mg, 0.12 mmol)] ; tetrakis(triphenylphosphine)palladium (0) [generated in situ from tris(dibenzylideneacetone)dipalladium chloroform adduct (27 mg, 0.025 mmol) and triphenylphosphine (52 mg, 0.20 mmol)]

With the complex challenges of chemical substances, we look forward to future research findings about 52522-40-4,belong catalyst-palladium compound

Reference£º
Patent; Universitetet i Olso; US2007/203159; (2007); A1;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

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

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.

With the complex challenges of chemical substances, we look forward to future research findings about Tris(dibenzylideneacetone)dipalladium-chloroform

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

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

General procedure: 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.

With the complex challenges of chemical substances, we look forward to future research findings about Tetrakis(triphenylphosphine)palladium

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

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

With the complex challenges of chemical substances, we look forward to future research findings about Tris(dibenzylideneacetone)dipalladium-chloroform

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

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: 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.

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

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

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

Solid [Pd(bpy)Cl2] (0.166 g, 0.5 mmol) was added to dl-H2pa (0.064 g, 0.5 mmol) in ethanol (8 mL) containing triethyl amine (0.05 g, 0.5 mmol). The mixture was stirred for 72 h. The yellow-beige precipitate was filtered off, washed with ethanol and air-dried. Yield: 45%. Anal. Calcd. for C16ClH22N3O4Pd: C, 41.6; H, 4.8; N, 9.1; Cl, 7.7; Pd, 23.0%, Found: C, 41.5; H, 4.4; N, 9.0; Cl, 7.6; Pd, 23.1%. Conductivity data (10-3 M in DMF):LambdaM = 97.0 ohm-1. IR (cm-1): nu(NH) 3106; nuas(COO-) 1659; nus(COO-) 1411; nu(Pd-O) 521; nu(Pd-N) 471 cm-1. Raman: nuas(COO-) 1598; nus(COO-) 1402; delta(NH) 1560; nu(Pd-O) 529; nu(Pd-N) 450 cm-1; 1H NMR (d6-DMSO/TMS, ppm), 3.73 (d, H, Halpha); 2.50 (m, 2H, Hbeta); 2.07 (m, 2H, Hgamma); 1.30 (m, 2H, Hdelta); 3.45, 3.10 (m, 2H, Hepsilon); 13.19 (s, H, NH), ESI-MS: m/z, 816.7 {Pd(Hpa)(bpy)]2Cl}+, 780.7 {[Pd(bpy)(Hpa)]2}+, 390.0 [Pd(bpy)(Hpa)]+, 263.0 [Pd(bpy)]+.

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

Reference£º
Article; Alie El-Deen, Afaf A.; El-Askalany, Abd El-Monem E.; Halaoui, Ruba; Jean-Claude, Bertrand J.; Butler, Ian S.; Mostafa, Sahar I.; Journal of Molecular Structure; vol. 1036; (2013); p. 161 – 167;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

As a common heterocyclic compound, it belongs to catalyst-palladium compound, name is Tris(dibenzylideneacetone)dipalladium-chloroform, and cas is 52522-40-4, its synthesis route is as follows.,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)]+.

With the rapid development of chemical substances, we look forward to future research findings about Tris(dibenzylideneacetone)dipalladium-chloroform

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

[1,1′-Bis(diphenylphosphino)ferrocene]dichloropalladium(II), cas is 72287-26-4, it is a common heterocyclic compound, the catalyst-palladium compound, its synthesis route is as follows.,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+)

72287-26-4 is used more and more widely, we look forward to future research findings about [1,1′-Bis(diphenylphosphino)ferrocene]dichloropalladium(II)

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