September 16, 2020 | Catalyst palladium

A new synthetic route of 72287-26-4

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

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

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., 72287-26-4

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

A new synthetic route of Tris(dibenzylideneacetone)dipalladium-chloroform

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

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)]+.

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

The origin of a common compound 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.

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

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).

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

The origin of a common compound about 14871-92-2

[(bpy)PdCl2] (0.332 g, 1 mmol) and Tl+L (0.475 g, 1 mmol) in 10 mL of dichloromethane were stirred for 18 h at room temperature. The resulting solution was filtered and evaporated to about 1 mL in volume. Then hexane (10 mL) was added to precipitate as a red-orange solid. The solid was repeatedly washed with diethyl ether (3 ¡Á 10 mL) and dried under vacuum to give the pure complex (0.297 g, 52.31% yield, and 1 mmol). Anal. Calc. (%) for C23H16ClN5O2PdS (568.9752): C, 48.61; H, 2.84; N, 12.32; Found (%): C, 48.59; H, 2.82; N, 12.29. TOF-MS: 532.0060 [M – Cl] +. FT-IR: 2152 (m, NCN) cm-1. 1H NMR (DMSO-d6): delta 7.16-7.20 (m, 2H, H-Ar), 7.49-7.51 (m, 2H, H-Ar), 7.65 (t, 1H, H-5, 3J 7.2), 7.74 (t, 1H, H-5′, 3J 7.2), 7.91-7.99 (m, 4H, H-Ar), 8.34-8.40 (m, 4H, H-Ar), 8.76 (d, 1H, H-6, 3J 7.2), 9.09 (d, 1H, H-6′, 3J 7.2). 13C NMR (DMSO-d6): delta 114.0 (NCN), 119.9, 121.9, 124.0, 125.9, 128.9, 133.1, 137.8, 143.0, 147.0, 149.0, 150.7, 157.9.

Reference£º
Article; Tabrizi, Leila; Zouchoune, Bachir; Zaiter, Abdallah; Inorganica Chimica Acta; vol. 499; (2020);,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method

The origin of a common compound about 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

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

A new synthetic route of Tris(dibenzylideneacetone)dipalladium-chloroform

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

The origin of a common compound about 12107-56-1

This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,12107-56-1,Dichloro(1,5-cyclooctadiene)palladium(II),its application will become more common.

A common heterocyclic compound, 12107-56-1,Dichloro(1,5-cyclooctadiene)palladium(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. 12107-56-1

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.

Reference£º
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

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).

Some scientific research about Tris(dibenzylideneacetone)dipalladium-chloroform

52522-40-4 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.

General procedure: 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

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

To a yellow suspension containing 0.20 g (0.60 mmol) of [Pd(bpy)Cl2] in water (20 mL)was added 0.08 g (0.60 mmol) of HaptHCl. After the mixture was stirred at 50 C for 7 h, theresulting yellow solution was filtered. To the yellow filtrate was added an aqueous solution ofNaClO4 (2 M, 10 mL), followed by standing at room temperature for 1 d. The resulting yellowcrystals of [1](ClO4)4 suitable for X-ray analysis were collected by filtration. Yield: 0.32 g (87%).

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