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Downstream synthetic route of Dichlorotris(triphenylphosphino)ruthenium (II)

The chemical industry reduces the impact on the environment during synthesis,15529-49-4,Dichlorotris(triphenylphosphino)ruthenium (II),I believe this compound will play a more active role in future production and life.

15529-49-4, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. Dichlorotris(triphenylphosphino)ruthenium (II), cas is 15529-49-4,the ruthenium-catalysts compound, it is a common compound, a new synthetic route is introduced below.

2-Methyl-acrylic acid 3-trimethoxysilane propyl ester (87 mg, 0.35 mmol) in dry THF was treated with triethylamine (0.20 mL) and the mixture was stirred for 30 min at ambient temperature under air. [RuCl2(PPh3)3] (335 mg, 0.35 mmol) was added and the reaction mixture was stirred at reflux for 2 h, during which there was a color residue was washed with diethyl ether and hexane. Recrystallization from CH2Cl2/hexane afforded dark green crystals of 1 in a week. Yield: 128 mg, 47% (based on Ru). IR (KBr disc, cm-1): nu(C=C) 1623 (s), nu(OCO) 1504 (s) and 1472 (s). MS (FAB): m/z = 781 [M]+, 746 [M-Cl]+, 711 [M-2Cl]+. mueff = 1.93 muB. Anal. for C40H35O2Cl2P2Ru: calcd. C 61.46, H 4.51%; found C 61.41, H 4.48%.

Reference£º
Article; Gu, Jiling; Shi, Li-Miao; Ma, Xiu-Fang; Jia, Ai-Quan; Zhang, Qian-Feng; Inorganica Chimica Acta; vol. 466; (2017); p. 382 – 388;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Downstream synthetic route of Dichlorotris(triphenylphosphino)ruthenium (II)

15529-49-4, In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles.,15529-49-4 ,Dichlorotris(triphenylphosphino)ruthenium (II), other downstream synthetic routes, hurry up and to see

As a common heterocyclic compound, it belongs to ruthenium-catalysts compound, name is Dichlorotris(triphenylphosphino)ruthenium (II), and cas is 15529-49-4, its synthesis route is as follows.

A 50 ml three-necked flask equipped with a stirring reflux device was charged with 1 mmol of 2-diphenylphosphineaniline,1.5 mmol of m-ethoxybenzyl alcohol, 1 mmol of bis (diphenylphosphinoethane), 1 mmol of RuCl2 (PPh3) 3, 1.5 mmol of sodium hydroxide and 20 ml of benzene at a temperature of 100 C for 24 h under a nitrogen atmosphere,After cooling and filtering, the obtained solid was recrystallized from a mixed solvent of CH 2 Cl 2 and petroleum ether to give product 4 in a yield of 86%.

Reference£º
Patent; Luoyang Normal College; Li Hongmei; Xu Chen; Zu Enpu; Xiao Zhiqiang; Han Xin; (12 pag.)CN104804048; (2017); B;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

The important role of 15529-49-4

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of Dichlorotris(triphenylphosphino)ruthenium (II), 15529-49-4

The complex RuCl2(PPh3)3 (4) (0.150 g, 0.156 mmol) suspended in 2 ml of distilled toluene, was reacted with HCNN-H (1) (36 mg, 0.174 mmol) and triethylamine (0.22 ml, 0.158 mmol). After stirring the mixture for 2 hours at 110 ?C the solution volume was reduced to about half and the complex was precipitated by adding 2 ml of pentane. The solid obtained was filtered off, washed with pentane (3 x 5 ml) and dried under reduced pressure. Yield 100 mg (74%). Elemental analysis (%) calculated for C50H41ClN2P2Ru. C, 69.16; H, 4.76; N, 3.23. Found: C, 69.35; H, 4.85; N, 3.34. 31P{1H} NMR (81.0 MHz, CD2Cl2, 20 C, H3PO4): delta 56.5 (d, J(PP) = 33.4 Hz), 50.5 (d, J(PP)= 33.4 Hz).

Reference£º
Patent; Universita’ Degli Studi di Udine; RIGO, Pierluigi; BARATTA, Walter; SIEGA, Katia; CHELUCCI, Giorgio Adolfo; BALLICO, Maurizio; MAGNOLIA, Santo; EP2178843; (2013); B1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

The important role of 15529-49-4

To a round-bottomed flask with a stir bar was placed with [Ru(PPh3)3Cl2] (868 mg, 2.0 mmol) under the nitrogen. Pre-dried THF(10 mL) was added and the resulting mixture was stirred at room temperature. Then salen-enH2 (536 mg, 2.0 mmol) and a little excess of Et3N (252 mg, 2.5 mmol) in THF (5 mL) were added. The reaction mixture was stirred at room temperature overnight. After removal of solvents, CH2Cl2 (15 mL) was added and the solution was filtered through cilite. The filtrate was concentrated and the residue was washed with Et2O (5mL 2) and hexane (5 mL 2) to give the desired product. Recrystallization from CH2Cl2/Et2O (1:2) afforded green block-shaped crystals of [RuCl(PPh3)(salen)] (3) suitable for X-ray diffraction in three days. Yield: 1011 mg, 76% (based on Ru). leff = 1.98 lB. IR (KBr disc, cm1):1599 (mCN), 1317 (mCAO), 1432, 1085 and 690 (mPPh3). MS (FAB):m/z 665 [M+], 630 [M+Cl], 403 [M+PPh3], 368 [Ru(salen-en)]+.Anal. Calc. for C34H29N2O2ClPRu (%): C, 59.97; H, 3.77; N, 6.36.Found: C, 60.05; H, 3.73; N, 6.39.

Reference£º
Article; Tang, Li-Hua; Wu, Fule; Lin, Hui; Jia, Ai-Quan; Zhang, Qian-Feng; Inorganica Chimica Acta; vol. 477; (2018); p. 212 – 218;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

The important role of 15529-49-4

N1-(2-aminoethyl)-1,2-ethanediamine (0.057 ml, 0.58 mmol) ligand was dissolved in 10 mL of dichloromethane and the solution was added dropwise to a stirred solution of [RuCl2(PPh3)3] (1) (0.500 g, 0.522 mmol) in 10 mL of dichloromethane. The reaction mixture was stirred approximately for 50 min at room temperature. The brown solution was filtered to remove the insoluble impurities. The solvent was reduced by a vacuum and the product was then precipitated by adding n-hexane. The yellow solid was filtered and washed three times with 20 mL of diethyl ether. Crystals suitable for X-ray structural analysis have been obtained by layer-diffusion of diethylether into dichloromethane solutions of the complex. Yield (0.342g, 82%). M.p is 239-241C. IR (KBr, nucm-1): 3330 (nuFree NH2), 3276 (nuNH2), 3227 (nuNH). 1H NMR (CD2Cl2, delta ppm): 2.48-4.21 (br, m, 13H, (H2NCH2CH2)2NH), 7.24-7.78 (m, 30H, C6H5). 31P{1H} NMR (CD2Cl2): delta (ppm) 44.00 and 43.94 (dd). FAB-MS: 799.2. Anal. Found: C, 60.22; H, 5.28; N, 5.14%. Calc. for C40H43Cl2N3P2Ru: C, 60.08; H, 5.42; N, 5.25.

Reference£º
Article; Al-Noaimi, Mousa; Nafady, Ayman; Warad, Ismail; Alshwafy, Rwaida; Husein, Ahmad; Talib, Wamidh H.; Hadda, Taibi Ben; Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy; vol. 122; (2014); p. 273 – 282;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Application of 15529-49-4

(PPh3)3RuCI2 (1 eq., 0.575 g, 0.6 mmol) and 1-(4-fluorophenyl)-1-phenylprop-2-yn-1-ol (compound 16A, 1.5 eq., 0.20 g, 0.9 mmol) were added in 4 ml HCI/dioxane solution (0.15 mol/l). The solution was heated to 90C for 3 hour, after which the solvent was removed under vacuum. Hexane (20 ml) was added to the flask and the solid was ultrasonically removed from the wall. The resulting suspension was filtered and washed two times using hexane (5 ml). The remaining solvent was evaporated affording a red-brown powder; 0.49 g (Yield: 90%). The product was characterized by NMR spectra 31P.31P NMR (121.49 MHz, CDCI3): 628.26.

Reference£º
Patent; GUANG MING INNOVATION COMPANY (WUHAN); W.C. VERPOORT, Francis; YU, Baoyi; WO2014/108071; (2014); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Application of (1,3-Bis(2,4,6-trimethylphenyl)-2-imidazolidinylidene)dichloro(phenylmethylene)(tricyclohexylphosphine)ruthenium

A 50 ml three-necked flask equipped with a stirring reflux device was charged with 1 mmol of 2-diphenylphosphineaniline, 1.5 mmol of p-bromobenzyl alcohol, 1 mmol of bis Dicyclohexylphosphine propane,mmol RuCl2 (PPh3) 3,1 mmol potassium hydroxide, 20 ml dioxane, the temperature was 110 C, heated for 20h under a nitrogen atmosphere, cooledHowever, filtration and recrystallization of the resulting solid from a mixed solvent of CH 2 Cl 2 and petroleum ether gave product 6 in a yield of 87%.

Some tips on Dichlorotris(triphenylphosphino)ruthenium (II)

As a common heterocyclic compound, it belongs to ruthenium-catalysts compound, name is Dichlorotris(triphenylphosphino)ruthenium (II), and cas is 15529-49-4, its synthesis route is as follows.

General procedure: A methanol (10ml) solution containing the appropriate N-S pro-ligand and triethylamine was refluxed under argon for 15min and then the complex [RuCl2(PPh3)3] was added. The resulting brown suspension was refluxed for 3h, to afford a yellow suspension. After cooling, the yellow solid was collected by filtration, washed with methanol (3¡Á5ml), and dried under reduced pressure. 2.6.2 [Ru(mcbtz)2(PPh3)2] (2) Hmcbtz (0.035 g – 2.0 * 10-4 mol); NEt3 (30 mul – 2.0 * 10-4 mol), and [RuCl2(PPh3)3] (0.095 g – 9.9 * 10-5 mol). Yield: 65 mg – 68.5%. 31P{1H} NMR (81 MHz, CDCl3) 52.2 ppm (s). 1H NMR (200 MHz, CDCl3), delta/ppm 8.0-6.5 (m, 30H Ph – PPh3 and 8H Ph – mcbtz-). Anal.exp. (calc. for C50H38N2P2RuS4) C-62.3 (62.7); H, 4.0 (4.0); N, 2.8 (2.9); S, 12.8(13.4).

Reference£º
Article; Appelt, Patricia; Fagundes, Francisco D.; Facchin, Gianella; Gabriela Kramer; Back, Davi F.; Cunha, Mario A.A.; Sandrino, Bianca; Wohnrath, Karen; De Araujo, Marcio P.; Inorganica Chimica Acta; vol. 436; (2015); p. 152 – 158;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

New learning discoveries about 15529-49-4

As a common heterocyclic compound, it belongs to ruthenium-catalysts compound, name is Dichlorotris(triphenylphosphino)ruthenium (II), and cas is 15529-49-4, its synthesis route is as follows.

A 50 ml three-necked flask equipped with a stirring reflux device was charged with 1 mmol of 2-diphenylphosphineaniline,2 mmol of benzyl alcohol, 1 mmol of bisdiphenylphosphinemethane, 1 mmol of RuCl2 (PPh3) 3,2 mmol of triethylamine, 20 ml of toluene, heating at 110 C. for 12 h under a nitrogen atmosphere, cooling,The resulting solid was recrystallized from a mixed solvent of CH 2 Cl 2 and petroleum ether to give product 1 in a yield of 89%.

New learning discoveries about 15529-49-4

It is a common heterocyclic compound, the ruthenium-catalysts compound, Dichlorotris(triphenylphosphino)ruthenium (II), cas is 15529-49-4 its synthesis route is as follows.

EXAMPLE B2Preparation of [(Cl)2Ru(Pphenyl3) (ligand L2)], K2 272.5 mg (0.284 mmol) of dichlorotris(triphenylphosphine)ruthenium(II) and 160.0 mg (0.296 mmol) of ligand L2 are placed in a 10 ml Schlenk tube and admixed with 6.5 ml of dry toluene under argon. The dark suspension is stirred overnight at room temperature, resulting in a colour change to orange-red. After addition of 4 ml of dry pentane, the stirrer is switched off and the supernatant orange solution is filtered off with suction from the orange solid. The solid is washed five times with 4 ml each time of pentane and dried in a high vacuum. This gives 244 mg (88% of theory) of the title compound as an orange powder. 31P-NMR (C6D6, 121.5 MHz, ppm): 49.7 (d, J=40), 61.2 (d, J=40).

Reference£º
Patent; Spindler, Felix; Nettekoven, Ulrike; Perseghini, Mauro; US2009/105481; (2009); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI