Extracurricular laboratory: Synthetic route of 50982-12-2

As the rapid development of chemical substances, we look forward to future research findings about 50982-12-2

Dichloro(cycloocta-1,5-diene)ruthenium(II), cas is 50982-12-2, it is a common heterocyclic compound, the ruthenium-catalysts compound, its synthesis route is as follows.

b) A brown suspension of RuCl2(1,5-cyclooctadiene) (560 mg; 2 mmol), 0.6 ml of 1,8-diazobicyclo[5.4.0]undec-7-ene (DBU) and 1.18 g of tricyclohexylphosphine in 60 ml of isopropanol was stirred at 80 C. for 2 hours. 60 ml of toluene was added to the resulting brick-red suspension and the mixture was stirred at 80 C. for a further 90 minutes and cooled to -10 C. After addition of 0.55 ml of trimethylsilylacetylene, 10 ml of 2 M HCl solution in diethyl ether were added and the mixture was subsequently stirred for 5 minutes. The mixture was warmed while stirring to 0 C. and stirred for 45 minutes. After evaporation at 0 C. in a high vacuum, the residue was stirred with cold MeOH. The resulting violet powder was washed with cold methanol and dried under reduced pressure. Yield 1.40 g (92%).

As the rapid development of chemical substances, we look forward to future research findings about 50982-12-2

Reference£º
Patent; Evonik Degussa GmbH; US2011/40099; (2011); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Brief introduction of 50982-12-2

As the paragraph descriping shows that 50982-12-2 is playing an increasingly important role.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.50982-12-2,Dichloro(cycloocta-1,5-diene)ruthenium(II),as a common compound, the synthetic route is as follows.

A mixture of (0421) [RuCl2(COD)]n (359 mg, 1.281 mmol), PPh3 (336 mg, 1.281 mmol) and ligand la (341 mg, 1.281 mmol) was stirred in THF (15 ml) at 75 C for 39 h in a KONTES pressure tube. After cooling down, the resulting brick precipitate was collected on a filter frit, washed with diethyl ether (3 >< 5 ml) and vacuum dried. Recrystallization from hot dichloromethane following layering with diethyl ether afforded analytically pure complex A-l in 29% yield (260 mg). As the paragraph descriping shows that 50982-12-2 is playing an increasingly important role. Reference£º
Patent; LOS ALAMOS NATIONAL SECURITY, LLC; DUB, Pavel, A.; GORDON, John, Cameron; WO2015/191505; (2015); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Application of 50982-12-2

As the rapid development of chemical substances, we look forward to future research findings about 50982-12-2

A common heterocyclic compound, the ruthenium-catalysts compound, name is Dichloro(cycloocta-1,5-diene)ruthenium(II),cas is 50982-12-2, mainly used in chemical industry, its synthesis route is as follows.

Next, 31.56 g of this (eta-1,5-cyclooctadiene)ruthenium(II) dichloride, 34.97 g of sodium carbonate, 28 mL of 2,4-pentanedione and 100 mL of N,N-dimethylformamide were placed in a nitrogen-flushed three-neck flask and stirred at 140 C. for 1 hour. Following reaction completion, the solution was cooled to room temperature, then alumina column chromatography (developing solvent: diethyl ether) was carried out. The resulting solution was concentrated, after which 120 mL of water was added and the solution was left at rest for 3 hours. The crystals that precipitated out were collected by filtration, and after being washed with water, were dried in vacuo. 46.53 g of bis(2,4-pentanedionato)(eta-1,5-cyclooctadiene)ruthenium(II) was obtained as an orangey-yellow solid. The yield was 94 wt %.

As the rapid development of chemical substances, we look forward to future research findings about 50982-12-2

Reference£º
Patent; JSR Corporation; US2012/282414; (2012); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Application of (R)-(+)-N,N-Dimethyl-1-ferrocenylethylamine

As the rapid development of chemical substances, we look forward to future research findings about 50982-12-2

The ruthenium-catalysts compound, name is Dichloro(cycloocta-1,5-diene)ruthenium(II),cas is 50982-12-2, mainly used in chemical industry, its synthesis route is as follows.

Separately, 200 ml of well dried tetrahydrofuran was fed to a 500 ml flask whose inside had been substituted by argon, and 5 g of dichloro(cyclooctadienyl)ruthenium was injected into the flask and well mixed with the above tetrahydrofuran to obtain a suspension. This suspension was cooled to -78 C. in a stream of argon, and 15 ml of the above synthesized tetrahydrofuran solution of trifluoromethyl cyclopentadienyl sodium was added dropwise to the suspension over 1 hour. The reaction mixture was further stirred at -78 C. for 3 hours and returned to room temperature under agitation over 12 hours. After the reaction mixture was let pass through a neutral alumina column in a stream of argon to be purified and concentrated, it was purified again by a neutral alumina column to obtain 0.2 g of bis(trifluoromethylcyclopentadienyl)ruthenium (yield rate of 30%).

As the rapid development of chemical substances, we look forward to future research findings about 50982-12-2

Reference£º
Patent; JSR Corporation; US2006/240190; (2006); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Application of (S)-4-Benzylthiazolidine-2-thione

As the rapid development of chemical substances, we look forward to future research findings about 50982-12-2

The ruthenium-catalysts compound, cas is 50982-12-2 name is Dichloro(cycloocta-1,5-diene)ruthenium(II), mainly used in chemical industry, its synthesis route is as follows.

A solution of (tBu2PCH2CH2)2NH (1 .0 g, 2.77 mmol) was added to [RuCl2(cod)]n (0.775 g, 2.77 mmol) and the resulting suspension stirred for 4 hours underargon. This was followed by the addition of 4-methoxyphenyl isonitrile (368 mg,2.77 mmol) and the mixture refluxed for 15 hours under argon. It was cooled to room temperature and ether (40 ml) added, and the suspension stirred for 1 hour at room temperature. It was filtered, washed with ether and dried under vacuum. Yield = 1 .44 g. X-ray quality crystals were obtained by slow diffusion of ether into a CH2CI2 solution of the compound.

As the rapid development of chemical substances, we look forward to future research findings about 50982-12-2

Reference£º
Patent; HADEED, Gerald, S.; ABDUR-RASHID, Kamaluddin; (61 pag.)WO2018/193401; (2018); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Introduction of a new synthetic route about Dichloro(cycloocta-1,5-diene)ruthenium(II)

With the rapid development of chemical substances, we look forward to future research findings about 50982-12-2

Dichloro(cycloocta-1,5-diene)ruthenium(II), cas is 50982-12-2, it is a common heterocyclic compound, the ruthenium-catalysts compound, its synthesis route is as follows.

A nitrogen-flushed three-neck flask was charged with 65.36 g of ruthenium trichloride trihydrate, 500 mL of ethanol and 250 mL of 1,5-cyclooctadiene, and the flask contents were refluxed under heating at 85 C. for 5 hours. Following the completion of refluxing, the solution was cooled to room temperature, after which filtration was carried out. The resulting solid was washed with 500 mL of diethyl ether and dried in vacuo, yielding 70.02 g of (eta-1,5-cyclooctadiene)ruthenium(II) dichloride as a brown solid. Next, 2.81 g of this (eta-1,5-cyclooctadiene)ruthenium(II) dichloride, 6.38 g of sodium carbonate, 2.9 mL of methyl 3-oxo-4,4,4-trifluorobutanoate and 10 mL of ethanol were placed in a nitrogen-flushed three-neck flask and refluxed under heating at 85 C. for 2 hours. Following the completion of refluxing, the solution was cooled to room temperature, then alumina column chromatography (developing solvent: acetone) was carried out. The resulting solution was concentrated and dried under reduced pressure, and 3.61 g of bis(methyl-3-oxo-4,4,4-trifluorobutanato)(eta-1,5-cyclooctadiene)ruthenium(II) was obtained as a black reddish-brown liquid. The yield was 66 wt %.

With the rapid development of chemical substances, we look forward to future research findings about 50982-12-2

Reference£º
Patent; JSR Corporation; US2012/282414; (2012); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Analyzing the synthesis route of 50982-12-2

As the paragraph descriping shows that 50982-12-2 is playing an increasingly important role.

50982-12-2, Dichloro(cycloocta-1,5-diene)ruthenium(II) is a ruthenium-catalysts compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Dichloro(1,5-cyclooctadiene)ruthenium (4.0 g, 0.014 moles), tricyclohexylphosphine (8.4 g, 0.030 moles), degassed triethylamine (2 mL), and degassed sec-butanol (60 mL) were combined in a pressure bottle under argon. The pressure bottle was purged with hydrogen gas, pressurized to 60 psi, and the mixture heated to 80 C. for 18 hours (the bottle was repressurized as needed to maintain 60 psi hydrogen). The reaction mixture was then allowed to cool down and the hydrogen gas was vented off. Degassed methanol (60 mL) was added to the orange slurry and the filtrate decanted off via stick filtration under argon to leave an orange solid in the bottle, which was washed with degassed methanol (60 mL). Degassed toluene (60 mL) was added to the orange solid and the orange slurry cooled to 0 C. Degassed 3-chloro-3-methyl-1-butyne (1.7 mL, 0.015 moles) was added dropwise via syringe at 0 C. The orange slurry progressively turned to a maroon slurry, while gas bubbled away. The mixture was stirred at room temperature for 2 hours after addition was complete. Ligand precursor [ 2] (18 g, 0.102 moles) was then charged and the mixture was heated to 80 C. and sparged with argon for 3 days (degassed toluene was added as needed). The brown slurry was allowed to cool to room temperature and a mixture of 30 mL methanol and 10 mL of concentrated hydrochloric acid was added in air with mixing. After stirring for 15 minutes at room temperature, the two phases were allowed to separate and the methanol phase was decanted off. Trituration with methanol (2¡Á50 mL) gave a solid, which was collected on a frit and washed with more methanol (2¡Á20 mL). The brown solid was then washed with hexanes (2¡Á20 mL) and dried to give [ 8] (5.1 g, 0.085 moles) in 61% yield.

As the paragraph descriping shows that 50982-12-2 is playing an increasingly important role.

Reference£º
Patent; MATERIA, INC.; Pederson, Richard L.; Woertink, Jason K.; Haar, Christopher M.; Gindelberger, David E.; Schrodi, Yann; (13 pag.)US9504997; (2016); B2;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Simple exploration of 50982-12-2

The synthetic route of 50982-12-2 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.50982-12-2,Dichloro(cycloocta-1,5-diene)ruthenium(II),as a common compound, the synthetic route is as follows.

0.25 g of metal sodium was mixed with well dried tetrahydrofuran in a 100 ml flask whose inside had been substituted by nitrogen and cooled to -78 C. A solution of 1.3 g of trimethylsilyl cyclopentadiene dissolved in 30 ml of tetrahydrofuran was added dropwise to the above solution in a stream of nitrogen over 1 hour and heated to room temperature under agitation over 3 hours to obtain a tetrahydrofuran solution of trimethylsilyl cyclopentadienyl sodium. Separately, 18 ml of a tetrahydrofuran solution (2.0 mol/l) of cyclopentadienyl sodium was prepared. Further separately, 5 g of dichloro(1,5-cyclooctadienyl)ruthenium was dissolved in 200 ml of well dried tetrahydrofuran in a 500 ml flask whose inside had been substituted by nitrogen. This solution was cooled to -78 C., and the above tetrahydrofuran solution of trimethylsilyl cyclopentadienyl sodium and the above tetrahydrofuran solution of cyclopentadienyl sodium were added dropwise to the solution at the same time in a stream of nitrogen over 1 hour. The resulting solution was stirred at -78 C. for 3 hours and heated to room temperature under agitation over 12 hours. After the resulting solution was let pass through a neutral alumina column in an argon gas atmosphere to be purified and concentrated, it was separated and purified by a neutral alumina column again to obtain 0.23 g of trimethylsilyl cyclopentadienyl(cyclopentadienyl)ruthenium (yield rate of 4.3%).

The synthetic route of 50982-12-2 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; JSR Corporation; US2006/240190; (2006); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Some tips on 50982-12-2

The synthetic route of 50982-12-2 has been constantly updated, and we look forward to future research findings.

50982-12-2, Dichloro(cycloocta-1,5-diene)ruthenium(II) is a ruthenium-catalysts compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A mixture of [RuCl2(COD)]n (309 mg, 1.103 mmol), PCy3 (309 mg, 1.103 mmol) and la (294 mg, 1.103 mmol) was stirred in toluene (10 ml) at 115 C for 48 h in a KONTES pressure tube. After cooling down, the brick colored precipitate was collected on a filter frit, washed with Et20 (3 x 10 ml) and vacuum dried to afford 642 mg of the crude material. To the crude material was added CH2C12 (~ 32 ml) and the obtained mixture was brought to reflux and filtered using a Whatman syringe filter (PTFE membrane, pore size 0.45 muiotaeta). Layering the obtained red-brown solution with Et20 (125 ml) afforded 327 mg (41%) of the product as a pink-brown powder after 5 days. Elem. Anal.: Calcd for C32H55Cl2N2OPRuS (718.81): C, 53.47; H, 7.71; N, 3.90%. Found: C, 53.11; H, 8.00; N, 3.86%. 31P{1H} (162 MHz, CD2C12, r.t.): delta 24.0 (s). 1H NMR (400 MHz, CD2C12, r.t.): delta 0.09 (brs, 1H), 0.92 (brs, 2H), 1.04-1.63 (m, 15H), 1.63-2.05 (m, 9H), 2.10-2.45 (brs, 3H), 2.45-2.70 (brs, 1H), 2.83-3.28 (overlapped, 7H), 3.31-3.56 (overlapped, 6H), 3.56-3.90 (overlapped, 4H), 3.98 (t, J~ 8 Hz, 1H), 5.57 (brs, NH, 1H), 7.31 (t, J~ 7 Hz, 2H), 7.38 (t, J~ 6 Hz, 1H), 8.15 (d, J~ 7 Hz, 2H). 13C{1H} selected for the coordinated NNS ligand (100.5 MHz, CD2C12, r.t.): delta 46.6 (s, 1C), 46.8 (s, 1C), 48.3 (s, 1C), 53.9 (s, 1C, overlapped with CD2C12 peak), 54.8 (s, 1C), 60.0 (s, 1C), 60.7 (s, 1C), 61.7 (s, 1C), 128.1 (s, 2Cmeta, Ph), 129.3 (s, Cpam, Ph), 134.9 (s, 2Cortho, Ph), 138.0 (s, Cipso, Ph).

The synthetic route of 50982-12-2 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; LOS ALAMOS NATIONAL SECURITY, LLC; DUB, Pavel, A.; GORDON, John, Cameron; WO2015/191505; (2015); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Brief introduction of 50982-12-2

As the paragraph descriping shows that 50982-12-2 is playing an increasingly important role.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.50982-12-2,Dichloro(cycloocta-1,5-diene)ruthenium(II),as a common compound, the synthetic route is as follows.

General procedure: The following common procedure was followed for the synthesesof complexes 1-5: A mixture of the ligand (0.36 mmol) and Ru(1,5-cod)Cl2(0.36 mmol) was dissolved in dry ethanol (10 ml) and the resultingmixture was refluxed for 2 h. The reaction volume was concentratedto a third of its original volume and the suspension was keptat 4 C overnight to give brick red solid which was filtered off,washed with cold ethanol and then diethyl ether. The solid wasdissolved in chloroform and excess of n-hexane was added toinduce the precipitation of the brick red solid product.2.3.1. [RuCl2(1,5cod) (L1)] (1)L1 (0.36 mmol, 66 mg) and Ru(1,5-cod)Cl2 (0.36 mmol,100 mg). Yield: 72% (120 mg). Mp. 220.0 C (dec. turns black withoutmelting). 1H NMR (400 MHz, CDCl3, 25 C, ppm) delta = 8.45 (s, 1H,imine CH), 8.25 (d, 1H, JH-H = 5.16 Hz, a proton of Py), 8.01-7.94(m, 2H, Py), 7.58-7.54 (m, 1H, Py), 7.82 (d, 2H, JH-H = 7.56 Hz,Ph), 7.39-7.34 (m, 3H, Ph), 4.75-4.74 (m, 2H, -CH, cod), 4.15-4.11 (m, 2H, -CH, cod), 2.74-2.57 (m, 4H, -CH2, cod), 2.20-2.14(m, 2H, -CH2, cod), 2.06-2.00 (m, 2H, -CH2, cod). 13C NMR(100 MHz, CDCl3, 25C, ppm) delta = 168.04 (imine C-H), 156.70(Py), 150.60 (Py), 149.44 (Py), 138.11 (Py), 135.94 (Py), 129.02(Ph), 128.93 (Ph), 127.88 (Ph), 127.80 (Ph), 120.81 (Ph), 92.25,91.87 (C, -CH, cod), 29.64, 29.22 (C, -CH2, cod). FT-IR (c/cm1):(cod, CC) 3038-2829 (m), (CN) 1594 (s), 1203 (s), 767 (s), 702(s). UV-Vis (dichloromethane, v/v): kmax (nm) = 229, 292, 345,439. HR-Mass (TOF MS ES+) C20H22N2Ru calculated: 393.0810,found: 393.0815. Anal. Calc. for C20H22Cl2N2Ru: C, 51.95; H, 4.80;N, 6.06. Found: C, 51.87; H, 5.10; N, 6.33.

As the paragraph descriping shows that 50982-12-2 is playing an increasingly important role.

Reference£º
Article; Thangavel, Saravanan; Rajamanikandan, Ramar; Friedrich, Holger B.; Ilanchelian, Malaichamy; Omondi, Bernard; Polyhedron; vol. 107; (2016); p. 124 – 135;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI