15529-49-4| Page 6 of 25 | Ruthenium catalysts

The important role of 15529-49-4

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.

(PPh3)3RuCI2 (1 eq., 0.575 g, 0.6 mmol) and 1-c-hexyl-1-phenyl-prop-2-yn-1-ol (compound E, 1.5 eq., 0.19 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; 0.51 g (Yield: 95 %). The product was characterized by NMR spectra 31P.31P NMR (121.49 MHz, CDCI3): 629.64.

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

Introduction of a new synthetic route about 15529-49-4

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.

RuCl2 (PPh3) 3 (800 mg, 0.83mmol) and (1R, 2R) -1, 2-diphenylethylenediamine (195 mg, 0.92 mmol) are weighed and charged into a 20-mL Schlenk flask. The flask was reduced pressure to degas therein and then nitrogen gas was introduced into the flask. Dichloromethane (8 mL) was added thereto through a syringe, and the mixture was stirred under nitrogen atmosphere at room temperature for 3 hours. The reaction solution was then Celite-filtered, and the Celite layer was washed with dichloromethane (2mL). The filtrate obtained was concentrated under reduced pressure to a volume of about 2 mL; hexane (16 mL) was added thereto; and the mixture was stirred at room temperature for 1 hour. The precipitate was collected by filtration under nitrogen atmosphere, and the powder obtained was dried under reduced pressure (1 mmHg), to give 531 mg of a desired product (yield: 70%).

Reference£º
Patent; Takasago International Corporation; EP1970360; (2008); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

The important role of 15529-49-4

With the complex challenges of chemical substances, we look forward to future research findings about Dichlorotris(triphenylphosphino)ruthenium (II)

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

General procedure: 1c (154 mg, 519 lmol) and [RuCl2(PPh3)3] (498 mg,519 lmol) were dissolved in CHCl3 (3 mL). The orange solutionwas stirred for 10 min at room temperature and then filteredthrough Celite. After four days, orange crystals, suitable for single-crystal X-ray diffraction, were obtained by vapor diffusion ofEt2O into the filtrate. The supernatant was decanted, the solidwas washed with Et2O (2 mL) and dried in vacuo. Yield: 312 mg(343 lmol, 66%).

With the complex challenges of chemical substances, we look forward to future research findings about Dichlorotris(triphenylphosphino)ruthenium (II)

Reference£º
Article; Gericke, Robert; Wagler, Joerg; Polyhedron; vol. 125; (2017); p. 57 – 67;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Application 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

RuCl2(PPh3)3 (1 g, 1 .04 mmol) and the ligand of formula (IVg) (obtained from Example 1 ) (231 .4 mg, 1 .1 mmol) were placed in a 25 mL Schlenk tube under argon atmosphere, and dissolved in dry diglyme (2 mL). The reaction mixture was heated to 165C for 2 h, allowed to cool down to room temperature and stored at -18C to precipitate further overnight. Cold Et2O (2 mL) was added while cooling with a dry ice//so-propa- nol bath. The precipitate was filtrated by cannula, and washed with Et2O (5 times 2 mL). The orange powder was dried in vacuo, affording 530 mg (79%) of Ru(6-MeNN- SEt)(PP i3)Cl2 as an orange powder. An equilibrium of two conformations of Ru(6- MeNNSEt)(PPh3)Cl2 are existent in solution, delivering a doubled set of signals in NMR. For 1H-NMR only data of the major conformation is given due to overlapping signals. 1H-NMR (300 MHz, CD2CI2): delta 7.67-7.16 (m, 17H, CHarom), 7.01 (d, 1 H, J = 7.8, CHarom), 5.65 (m, 2H), 4.47 (m, 1 H), 3.5 (m, 1 H), 3.34 (m, 1 H), 3.22 (d, 1 H, J = 1 1 .1 ), 2.98 (m, 1 H), 2.59 (m, 1 H), 1 .53 (m, 2H), 0.87 (t, 3H, J = 7.5) ppm. 31P-NMR (122 MHz, CD2CI2): delta 48.8, 45.8 ppm. HRMS (ESI+): calculated for C29H32CI2N2PRUS (M+H): 644.0518; found 644.0518 (M+H), 667.0412 (M+Na)

Reference£º
Patent; DSM IP ASSETS B.V.; BELLER, Matthias; BONRATH, Werner; DE VRIES, Johannes, Gerardus; FAN, Yuting; HUeBNER, Sandra; LEFORT, Laurent; MEDLOCK, Jonathan, Alan; PUYLAERT, Pim; VAN HECK, Richard; (65 pag.)WO2017/194662; (2017); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

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

Downstream synthetic route of 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.

A Schlenk flask was loaded with [Ru(PPh3)3(Cl)2] (2.0270 g,2.114 mmol) and bis(3-aminopropyl)phenylphosphine (1) (0.4816 g,2.147 mmol), to which was added 17 ml of anhydrous toluene to generate a yellow suspension. The mixture was stirred in an oil bath at 110 C, for two hours. The yellow suspension was then stirred for 16 h at room temperature, after which time the solid was isolated via canula filtration and washed with 100 ml of anhydrous diethyl ether 3 times. The solid was dried under vacuum for 72 h. Isolated mass 1.20 g, 86% yield. NMR data – 1H NMR (CDCl3, delta): 7.71 (m with appearance of t,6 H) 7.43 (m with appearnce of t, 2 H), 7.14-6.94 (m, 10 H), 6.88 (mwith appearance of t, 2 H) 4.25, (br, 2H, NH), 3.39 (br, 2H, NH and CH),3.08 (br, 1H, CH), 2.23-1.81 (m, 10H, 9CH and NH), 0.68 (br, 1H, CH). 13C{1H} NMR (CDCl3, delta): 138.7 (d, i-C of PPh), 137.0 (d, i-C of PPh3),134.0 (d, o-C of PPh3), 131.2 (d, o-C of PPh), 128.4 (s, p-C of PPh3),128.2 (s, p-C of PPh), 127.7 (d, m-C of PPh), 127.5 (d, m-C of PPh3),42.3, 40.5, 33.3 (d, 1JPC=26.9 Hz), 27.9 (d, 1JPC=27.8 Hz), 26.1,25.4. 31P{1H} NMR (CDCl3, delta): 48.8 (d, 2JPP=34 Hz), 32.65 (d,2JPP=34 Hz). Elemental analysis calculated (%) for C30H36Cl2N2P2Ru:C 53.93, H 5.51, N 4.25; found: C 53.72, H 5.51, N 4.52 Product is soluble in dichloromethane and chloroform, but insoluble in methanol,ethanol, isopropanol and acetonitrile. The product is air sensitive in solution, turning green on exposure to air. A sample of the solid exposed to air for 2 h and returned to the glove box was analysed by NMR; no new unassigned signals were observed in either the 1H or 31P NMR spectra. Single crystals of [Ru(1)PPh3(Cl)2] were grown by layering hexane onto a DCM solution of the complex to enable slow diffusion of the solvents

Reference£º
Article; Braden, Drew J.; Cariou, Renan; Shabaker, John W.; Taylor, Russell A.; Applied Catalysis A: General; vol. 570; (2019); p. 367 – 375;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Some tips on 15529-49-4

(PPh3)3RuCI2 (1 eq., 0.575 g, 0.6 mmol) and 1-(i-propyl)-1-phenylprop-2-yn-1-ol (compound 18A, 1.5 eq., 0.144 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; 0.48 g (Yield: 93%). The product was characterized by NMR spectra 31P.31P NMR (121.49 MHz, CDCI3): 629.55.

Introduction of a new synthetic route about 15529-49-4

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

An anhydrous Et2NH (10 mL) solution of dicyclohexylphosphinomethylpyridine-borane complex (280 mg, 0.923 mmol) was heated at 65C for 48 h under Ar. The solution was cooled to room temperature and Et2NH was removed in vacuo (ca. 10 mmHg, room temperature). To the residue was added sequentially dichlorotris(triphenylphosphino)ruthenium (II) (442.5 mg, 0.46 mmol) and an anhydrous toluene (10 mL). The resulting mixture was heated at 110C for 5 h under Ar, and was cooled to room temperature. Then to the mixture was added an anhydrous hexane (20 mL) to afford the yellow suspension. The mixture of the suspension was stirred at room temperature for 12 h and filtered through a filtration paper. The obtained yellowish orange solid was dried in vacuo (ca. 0.1 mmHg, room temperature) and dissolved in CH2Cl2. This solution was purified by column chromatography on silica gel (EtOAc/hexane =1/4) to afford RUPCY (1a) as orange powder (237 mg, 68%).

Reference£º
Article; Miura, Takashi; Held, Ingmar E.; Oishi, Shunsuke; Naruto, Masayuki; Saito, Susumu; Tetrahedron Letters; vol. 54; 21; (2013); p. 2674 – 2678;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

The important role of 15529-49-4

With the complex challenges of chemical substances, we look forward to future research findings about Dichlorotris(triphenylphosphino)ruthenium (II)

Step 4: (PPh^2CI2Ru(3-2-methylphenyl-5-methylphenyl-inden-1 -ylidene) (1 D): (PPh3)3RuCl2 (1 eq., 0.575 g, 0.6 mmol) and 1 ,1 -bis-2-methylphenyl-prop-2-yn-1-ol (compound C, 1.5 eq., 0.213 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; 0.52 g (Yield: 95 %). The product was characterized by NMR spectra H and 3 P. H NMR (300 MHz, CDCI3, TMS): delta 7.56 (dd, 1 1 H), 7.37 (t, 6 H), 7.21 -7.31 (m, 13 H), 7.09 (tetra, 3 H), 6.95 (t, 3 H), 6.47 (t, 1 H), 6.14 (s, 1 H), 2.20 (s, 3 H), 1 .66 (s, 3 H). 3 P NMR (121.49 MHz, CDCI3): delta 29.33.

With the complex challenges of chemical substances, we look forward to future research findings about Dichlorotris(triphenylphosphino)ruthenium (II)

Reference£º
Patent; GUANG MING INNOVATION COMPANY (WUHAN); W.C. VERPOORT, Francis; (69 pag.)WO2016/242; (2016); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Share a compound : 15529-49-4

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

General procedure: 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).

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

Extracurricular laboratory: Synthetic route of 15529-49-4

To Hpytol (0.12 g,0.5 mmol) in methanol (10 mL), [RuCl2(PPh3)3] (0.23 g, 0.25 mmol) in methanol (5 mL) was added. The reaction was carried out in presence of Et3N (0.05 mL, 0.5 mmol). The mixture was heated under reflux for 1.5 h, during which a deep red precipitate was obtained. It was filtered off, washed with methanol and ether, then dried in vacuo, Yield, 88%; mp 300 C. LM inCH2Cl2 3 U1 cm2 mol1. Elemental Anal. Calcd. ForC66H60N4O4RuP2: C, 69.7; H, 5.3; N, 4.9%. Found: C, 69.5; H, 5.0; N,4.8%. IR (KBr, cm1): n (OeH) 3407(m,b), n (C]N) 1625, n (CeO)1285(s), n(PPh3) 1091(s), n(RueO) 522(m), n (RueN) 460 (m). 1HNMR (DMSO-d6,d/ppm): 8.57 (HC]N), 1H, s); 8.1(H6), 1H, s);7.33e7.44 (Ph-H, 4H, m); 5.07 (CH2, 2H, s); 4.37 (OHCH2OH, 1H, s);2.3 (CH3, 3H, s).

Reference£º
Article; Elsayed, Shadia A.; Noufal, Aya M.; El-Hendawy, Ahmed M.; Journal of Molecular Structure; vol. 1144; (2017); p. 120 – 128;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI