15529-49-4| Ruthenium catalysts

Some tips on 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.

To a solution of N,O-LH-Cl (930?mg, 4.0?mmol) in THF (20?mL) was added [Ru(PPh3)3Cl2] (868?mg, 2.0?mmol), which was then stirred under N2 for 15?min. Triethylamine (Et3N) (404?mg, 4.0?mmol) was introduced, and the reaction mixture was stirred overnight at room temperature, during which the color of solution changed from brown to dark green. After removal of solvents in vacuo, the residue was extracted with CH2Cl2 (5?mL?*?2) and the solution was filtered. The filtrate was layered with Et2O (20?mL) at room temperature, and dark green block-shaped crystals of cis-[RuCl(PPh3)(kappa2-N,O-L-Cl)2] (1) were harvested in three days. Yield: 1187?mg, 69% (based on Ru). mueff?=?1.98?muB. IR (KBr disc, cm-1): 1592 (nuC=N), 1314 (nuC-O), 1437, 1092 and 698 (nuPPh3). MS (FAB): m/z 860 [M+], 825 [M+-Cl], 598 [M+-PPh3], 563 [Ru(kappa2-N,O-L-Cl)2]+. Anal. Calc. for C44H33N2O2Cl3PRu(%): C, 61.44; H, 3.87; N, 3.26. Found: C, 61.47; H, 3.83; N, 3.24.

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

Analyzing the synthesis route 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

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: Synthesis of the ruthenium(II) Schiff base complexes (2a-d) was accomplished according to the following procedure: To a solution of Schiff base 1a-d in methanol was added dropwise a solution of NaOH in methanol and the reaction mixture was stirred for 2hat room temperature. The deprotonated ligand mixture was transferred by cannula to a 50-mL three-necked flask fitted with a reflux condenser containing the [RuCl2(PPh3)3] precursor, stirred mixture was refluxed for 4h. A yellow precipitate was then filtered and washed with methanol and ethyl ether and then dried in a vacuum.

Reference£º
Article; Afonso, Maria Beatriz A.; Cruz, Thais R.; Silva, Yan F.; Pereira, Joao Clecio A.; Machado, Antonio E.H.; Goi, Beatriz E.; Lima-Neto, Benedito S.; Carvalho-Jr, Valdemiro P.; Journal of Organometallic Chemistry; vol. 851; (2017); p. 225 – 234;,
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

To a slurry of HimtMPh (38 mg, 0.20 mM) and MeONa (10.8 mg, 0.20 mM) in tetrahydrofuran(THF) (5 mL) was added a solution of [RuCl2(PPh3)3] (96 mg, 0.10 mM) in THF(10 mL). The mixture was stirred for 8 h at room temperature. The solvent was removed invacuo, and the residue was washed with hexane. The residue was extracted with dichloromethaneand filtered; the solvent was removed in vacuo and further recrystallized fromCH2Cl2/EtOH/Et2O at room temperature. Block orange crystals of 1¡¤EtOH suitable for Xraydiffraction were obtained in a week. Yield: 90 mg, 86%. 31P NMR (CDCl3): 29.2, 55.6 ppm. 1H NMR (CDCl3): 1.25 (EtOH), 2.35 (s, Me, 6H), 3.72 (EtOH), 6.31 (s, imt-CH, 2H), 6.50 (d, imt-CH, J = 1.6 Hz, 2H), 6.96-6.70 (m, 12H), 7.09-7.13 (m, 6H), 7.19(d, C6H4, J = 8.0 Hz, 4H), 7.26-7.30 (m, 16H) ppm. IR (KBr disk, cm1): 3052 (w), 1634(m), 1595 (m), 1499 (s), 1432 (s), 1362 (s), 1263 (s), 1098 (s), 1031 (s), 805 (s), 694 (s),538 (s), 524 (s), 500 (m). MS (FAB): m/z 1052 [M+], 790 [M+ – PPh3], 528 [M+ -2PPh3]. Anal. Calcd for C56H48N4P2S2Ru¡¤(C2H6O) (%): C, 66.20; H, 5.36; N, 5.32.Found: C, 66.11; H, 5.34; N, 5.35

Reference£º
Article; Qin, Yi; Ma, Qing; Jia, Ai-Quan; Chen, Qun; Zhang, Qian-Feng; Journal of Coordination Chemistry; vol. 66; 8; (2013); p. 1405 – 1415;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

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Introduction of a new synthetic route about Dichlorotris(triphenylphosphino)ruthenium (II)

General procedure: Diphosphine ligand (2.0 mmol) was dissolved in 10 mL of dichloromethane and the solution was added dropwise to a stirred solution of RuCl2(PPh3)3 (1.0 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.

Reference£º
Article; Al-Noaimi, Mousa; Warad, Ismail; Abdel-Rahman, Obadah S.; Awwadi, Firas F.; Haddad, Salim F.; Hadda, Taibi B.; Polyhedron; vol. 62; (2013); p. 110 – 119;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

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.

A 50 ml three-necked flask equipped with a stirring reflux device was charged with 1 mmol of 2-diethylphosphine aniline,1.6 mmol of m-methylbenzyl alcohol, 1 mmol of 1,1′-dimethylphosphine ferrocene, 1 mmol of RuCl2 (PPh3) 3, 1.5 mmol of triethylamine and 20 ml of toluene at a temperature of 110 C. for 20 h under a nitrogen atmosphereAfter cooling, filtration and recrystallization of the resulting solid from a mixed solvent of CH 2 Cl 2 and petroleum ether, product 18 was obtained in a yield of 83%.

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

Introduction of a new synthetic route 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.

To a solution of [Ru(PPh3)3Cl2] (868?mg, 2.0?mmol) in THF (10?mL) was added a solution of N,O-LH-NO2 (972?mg, 2.0?mmol) and Et3N (404?mg, 4.0?mmol) in EtOH (5?mL), and then the mixture was heated at 90?C with stirring overnight, during which there was a color change from brown to green. After removal of solvents in vacuo, the residue was extracted with CH2Cl2 (5?mL?*?2) and the solution was filtered. The clearly green filtrate was layered with Et2O (20?mL) at room temperature, and dark green block-shaped crystals of trans-[RuCl(PPh3)(kappa2-N,O-L-NO2)2]¡¤Et2O (2) were obtained in three days. Yield: 1356?mg, 71% (based on Ru).

The important role of 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.

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).

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Compound 6 (604.4 mg, 1.0 mmol) and degassed morpholine (20 mL) were placed in a 100-mL Young-Schlenk container substituted with argon gas. Thereafter, the Young-Schlenk container was placed in an oil bath, and heated to 120 C. while stirring the components in the Young-Schlenk container, thereby causing a reaction. The progress of the reaction was confirmed by TLC, and the heating was stopped after two hours. Subsequently, the morpholine in the reaction mixture restored to room temperature (25 C.) was removed after collection with a liquid nitrogen trap under reduced pressure (0.1 to 2 mmHg). At this time, the reaction mixture was sufficiently stirred, and the Young-Schlenk container was immersed in water at room temperature (25 C.) to prevent cooling of the Young-Schlenk container by the heat of vaporization. (0217) After sufficiently removing the morpholine, dichlorotris(triphenylphosphino)ruthenium (II) (958.8 mg, 1.0 mmol) and dehydrated toluene (20 mL) were added while introducing argon gas into the container, and the mixture was heated to 110 C. using an oil bath, thereby causing a reaction. The heating was stopped after three hours, and the reaction mixture was restored to room temperature (25 C.). (0218) Subsequently, dehydrated hexane (40 mL) was added to the reaction mixture in an argon gas atmosphere. Thereafter, the whole mixture, including the hexane layer and the toluene layer, in the Young-Schlenk container was stirred and completely mixed. After leaving the mixture unattended for 15 minutes, the generated purple substance was filtered out in an argon atmosphere while being washed with dehydrated diethylether, thereby obtaining a crude product. (0219) Subsequently, the resulting crude product was subjected to column chromatography (developing solvent: chloroform/ethyl acetate=5/1) in which silica gels were accumulated to about 10 cm, thereby removing a compound with high polarity. The effluent was collected to a flask and the collection was continued until the color of the purple liquid was slightly diluted. After this operation, the solution collected in the recovery flask was rapidly concentrated by an evaporator, thereby obtaining 435.1 mg (0.58 mmol, 58%) of substantially pure Compound 2c (RUPCY2) as a purple substance. (0220) The spectral data of Compound 2c (RUPCY2) is shown below. (0221) 1H NMR (500 MHz, CDCl3): delta 7.86 (d, 2H, J=7.4 Hz, C10H6N2), 7.66 (t, 2H, J=7.5 Hz, C10H6N2), 7.56 (d, 2H, J=7.5 Hz, C10H6N2), 3.87 (d, 4H, J=8.1 Hz, PCH2), 2.41 (br, 4H, C6H11), 2.18 (d, 4H, J=12.1 Hz, C6H11), 2.05 (d, 4H, J=10.9 Hz, C6H11), 1.54-1.81 (m, 20H, C6H11), 1.20-1.34 (m, 20H, C6H11). 13C NMR (150 MHz, CDCl3): delta 163.3, 158.3, 134.1, 122.0, 119.9, 40.5 (d, 1JPC=13.0 Hz), 36.3, 30.3, 29.4, 27.7, 27.5, 26.4. 31P{1H} NMR (241 MHz, CDCl3): delta 54.1. HRMS (ESI, (M-Cl)+) Calcd for C36H54ClN2P2Ru+: 713.2494. Found m/z=713.2476. (0222) FIG. 1 shows a result of X-ray single crystal structural analysis (Oak Ridge Thermal Ellipsoid Plot) of Compound 2c.

Reference£º
Patent; National University Corporation Nagoya University; Saito, Susumu; Noyori, Ryoji; Miura, Takashi; Naruto, Masayuki; Iida, Kazuki; Takada, Yuki; Toda, Katsuaki; Nimura, Sota; Agrawal, Santosh; Lee, Sunkook; (42 pag.)US9463451; (2016); B2;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

The important role of 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: The amine (4-CH3-pip, 4-CH2Ph-pip or 4-CH2(OH)-pip;0.34 mmol) was added to a solution of [RuCl2(PPh3)3] (0.26 mmol;0.25 g) in acetone (40 mL). The resulting dark green solution wasstirred for 2 h at RT. A green precipitate was formed, filtered,washed with methanol and ethyl ether, and then dried in vacuum.Complex 3 (R = OH): 67% yield. Analytical data for RuCl2P2NC42H43O are 62.15C, 5.34H, and 1.73% N; found 62.19C, 5.26H, and 1.83% N. FTIR in CsI: 323 for cm-1 for nu(Ru-Cl); 3230 cm-1 nu(N-H). 31P{1H} NMR in CDCl3: 62.7 ppm (s).

Reference£º
Article; Chaves, Henrique K.; Ferraz, Camila P.; Carvalho Jr., Valdemiro P.; Lima-Neto, Benedito S.; Journal of Molecular Catalysis A: Chemical; vol. 385; (2014); p. 46 – 53;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI