Month: August 2020

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.,50982-12-2

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 tetrahydrofuran to obtain a suspension. This suspension was cooled to -78 C. in a stream of argon, and 14 ml of a tetrahydrofuran solution of the above synthesized fluorocyclopentadienyl sodium was added dropwise to the above suspension over 1 hour. The obtained 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 0.4 g of bis(fluorocyclopentadienyl)ruthenium (yield rate of 8.4%).

With the rapid development of chemical substances, we look forward to future research findings about Dichloro(cycloocta-1,5-diene)ruthenium(II)

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

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.,50982-12-2

A mixture of [RuCl2(COD)]n (309 mg, 1.103 mmol), PCy3 (309 mg, 1.103 mmol) and Id (248 mg, 1.103 mmol) was stirred in toluene (10 ml) at 115 C for 48 h (in a KONTES pressure tube). After cooling, the brick colored precipitate was filtered on a filter frit, washed with Et20 (3 x 10 ml) and partially vacuum dried on the filter (vacuum pump). The residue was extracted from the filter frit with dichloromethane (6 >< 3 ml). The obtained solution was layered with Et20 (100 ml). Red-brown crystals were collected in few days (521 mg, 70%> yield). Elem. Anal: Calcd for (0461) C30H53Cl2N2PRuS (676.77): C, 53.24; H, 7.89; N, 4.14%. Found: C, 53.10; H, 7.95; N, 4.05%. 31P{1H} (162 MHz, CDC13, r.t.): delta 27.0 (s). 1H NMR (400 MHz, CDC13, r.t.): delta 0.78-3.90 (overlapped m, 47H), 5.57 (brs, 1H, NH), 7.22-7.53 (m, 3Eta), 8.10-8.30 (m, 2Eta). 13C{1H} (100.5 MHz, CDC13, r.t., selected without PCy3 carbon atoms): delta 46.7 (s, 1C), 46.8 (s, 1C), 48.5 (s, 1C), 52.3 (s, 1C), 54.2 (s, 1C), 67.2 (s, 1C), 128.2 (s, 2Cmeta, Ph), 129.4 (s, Cpara, Ph), 134.9 (s, 2Cortho, Ph), 137.8 (s, Cipso, Ph).

With the rapid development of chemical substances, we look forward to future research findings about Dichloro(cycloocta-1,5-diene)ruthenium(II)

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

Ruthenium(III) chloride hydrate, cas is 20759-14-2, it is a common heterocyclic compound, the ruthenium-catalysts compound, its synthesis route is as follows.,20759-14-2

(4) Preparation of trans-3′-oxospiro[cyclohexane-1,1′(3’H)-isobenzofuran]-4-carboxylic acid A mixture of 4-hydroxymethylspiro[cyclohexane-1,1′(3’H)-isobenzofuran]-3’one (190 mg), chloroform (2.0 mL), acetonitrile (2.0 mL) and sodium phosphate buffer (pH6.5, 2.0 mL) was cooled to 0 C., to which sodium periodate (612 mg) and ruthenium(III) chloride n-hydrate (10 mg) were added and the mixture was stirred for 30 minutes. The reaction mixture was stirred together with 1N hydrochloric acid (2.0 mL) for 30 minutes and partitioned between water (50 mL) and ethyl acetate (50 mL). The organic layer was washed with saturated saline solution, dried over anhydrous Na2SO4 and then concentrated. The residue was purified by column chromatography on silica gel (chloroform/methanol=100/1) to give the subject compound (98.6 mg).

With the rapid development of chemical substances, we look forward to future research findings about Ruthenium(III) chloride hydrate

Reference£º
Patent; Banyu Pharmaceutical Co., Ltd.; US6803372; (2004); B2;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

As a common heterocyclic compound, it belongs to quinuclidine compound,Quinuclidine-4-carboxylic acid hydrochloride,40117-63-3,Molecular formula: C8H14ClNO480,mainly used in chemical industry, its synthesis route is as follows.,301224-40-8

Potassium 2,4,6-triphenylthiophenolate 2d (53 mg, 0.14 mmol) was transferred to a 25 mL Schlenk flask, followed by addition of 5 mL of THF under argon, and the mixture was stirred vigorously and heated at 55 C. Hoveyda-Grubbs second generation catalyst (82 mg, 0.13 mmol) dissolved in toluene (1 mL) was then added, and the mixture stirred at 55 C. for 2.5 h. The solvents were then removed in vacuo, and the product was redissolved in 6 mL Et2O. Following filtration, 3 mL of hexane was added, and the mixture cooled to -40 C., causing precipitation of impurities. After allowing solids to settle, the solution was filtrated, and the solvents removed in vacuo to yield the crude 4d complex as a green powder (50.7 mg, 42%). 1H NMR (400.13 MHz, C6D6): delta=14.50 (s, 1H), 7.80 (d, J=6.4 Hz, 2H), 7.47 (t, J=6.7 Hz, 2H), 7.42-7.34 (m, 2H), 7.31-7.21 (m, 3H), 7.11 (t, J=7.2 Hz, 3H), 7.08-7.00 (m, 3H), 6.99-6.90 (m, 3H), 6.87 (s, 2H), 6.79-6.60 (m, 4H), 6.15 (d, J=8.2 Hz, 2H), 4.15 (sept, J=6.1 Hz, 1H), 3.38-3.20 (m, 4H), 2.47 (s, 6H), 2.38 (s, 6H), 2.29 (s, 6H), 1.15 (d, J=6.1 Hz, 3H), 0.59 (d, J=6.1 Hz, 3H). (0132) 13C NMR (100.6 MHz, CD2Cl2): delta=276.55, 210.42, 153.68, 146.72, 138.75, 138.16, 131.23, 129.58, 129.12, 128.97, 128.75, 128.31, 127.87, 127.77, 127.50, 127.23, 127.01, 125.83, 122.65, 121.72, 113.38, 76, 15, 53, 87, 51, 98, 21.54, 21.25, 20.83, 19.92, 19.04. MS (DART), m/z: 928.27512 (M+H)+; calc. for C55H56OClN2SRu: 928.27671.

With the synthetic route has been constantly updated, we look forward to future research findings about (1,3-Dimesitylimidazolidin-2-ylidene)(2-isopropoxybenzylidene)ruthenium(VI) chloride,belong ruthenium-catalysts compound

Reference£º
Patent; Bergen Teknologioverforing AS; Jensen, Vidar R.; Occhipinti, Giovanni; Hansen, Frederick Rosberg; US8716488; (2014); B2;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

As a common heterocyclic compound, it belong ruthenium-catalysts compound,(1,3-Dimesitylimidazolidin-2-ylidene)(2-isopropoxybenzylidene)ruthenium(VI) chloride,301224-40-8,Molecular formula: C31H38Cl2N2ORu,mainly used in chemical industry, its synthesis route is as follows.,301224-40-8

In a Schlenk flask, (H2IMes)Cl2Ru(CH-o-OiPrC6H4) (106 mg, 0.169 mmol, 1 eq) was dissolved in degassed CH2Cl2 (18 mL). 5,7-Dichloro-8-hydroxyquinoline (707 mg, 3.303 mmol, 19 eq) and Cs2CO3 (150 mg, 0.461 mmol, 16 eq) were added. The reaction mixture was stirred in a Schlenk flask under argon atmosphere overnight. (0099) The insoluble residue was filtered over celite. According to a TLC (CH/EE 5:1) two derivatives were formed. The products were separated via column chromatography (CH/EE 5:1) and fully characterized by NMR and crystal structure analysis. Yield=83% (46.5 mg 3 and 91 mg 4). (0100) 3: 1H-NMR (delta, 20 C., CDCl3, 300 MHz): 19.10 (s, 1H, Ru?CH), 8.09 (d J=4.04, 1H, CHhq), 7.95 (d J=8.56; j=1.43, 1H, CHhq), 7.68 (d J=8.43 j=1.30, 1H, CHPhq), 7.49 (s, 1H, CHhq), 7.17 (s, 1H, CHhq), 7.05 (m, 2H, CHhq), 6.56 (d J=8.04, 1H, CHhq), 6.48 (s, 2H, CHmes), 6.43 6,39 (?, 2H, CHph), 6.14 (s, 2H, CHmes), 6.06 (2H, CHhq+ph), 3.97 (5H, CH2+CHisoprop), 2.45 (s, 6H), 2.27 (s, 6H), 1.90 (s, 6H, CH31, 1?, 2, 2?, 3, 3?), 1.43 (d, 3H, CH3isoprop), 1.05 (d, 3H, CH3isoprop). (0101) 3: 13C-NMR (delta, 20 C., CDCl3, 75 MHz): 338.6 (1C, Ru?CH), 227.6 (1C, Ru-C), 162.6, 161.3, 149.7, 149.4, 149.0, 144.2, 143.2, 142.4, 142.3, 138.1 (Cq), 136.9 (Cq), 136.6 (Cq), 135.8 (Cq), 132.3 (CH), 131.7 (CH), 129.3 (CH), 129.2 (CH), 128.7, 127.7 (CH), 126.2, 125.8, 125.7, 122.2 (CH), 121.6 (CH), 121.0 (CH), 119.5 (CH), 118.9, 112.0, 109.2, 76.2 (1C, CHisoprop), 51.6 (2C, CH2-N), 23.1 (1C, CH3isoprop), 21.5 (1C, CH3isoprop), 20.8, 18.8, 18.5 (2C, CH3mes 7, 7?, 8, 8?, 9, 9?). (0102) 4: 1H-NMR (delta, 20 C., CDCl3, 300 MHz): 18.23 (bs, 1H, Ru?CH), 9.00 (d j=4.67 Hz, 1H, CHhq 1), 8.09 (d J=8.56 Hz, 1H, CHhq 3), 7.83 (d J=8.30 Hz, 1H, CHhq 3) 7.57 (s, 1H, CHhq 4 or 4), 7.12 (s, 1H, CHhq 4 or 4), 7.06 (q, 1H, CHhq 2), 6.94 (t, 1h; CHph 3 or 4), 6.59 (s, 2H, CHmes 3+3? or 5+5?), 6.39 (d, 1H, CHph 2 or 5), 6.26 (s, 2H, CHmes 3+3? or 5+5?), (d, 1H, CHph 2 or 5), (t, 1H, Chhq 2), 5.98 (t, 1H, CHph 3 or 4), 5.32 (d j=4.54 Hz, 1H, CHhq 1), 4.54 (m, 1H, CHisoprop), 3.92 (q, 4H, CH2mes), 2.57 (s, 6H), 2.04 (s, 6H), 1.91 (s, 6H, CH3mes 7, 7?, 8, 8?, 9, 9?), 1.53 (d, 3H, CH3isoprop), 1.31 (d, 3H, CH3isoprop). (0103) 13C-NMR (delta, 20 C., CDCl3, 75 MHz): Ru?C not observed, 209.5 (1C, Ru-C), 166.4 (Cq), 160.9 (Cq), 147.7 (Cq), 146.7 (Cq), 147.1 (Cq), 146.7 (Cq), 164.5 (CH), 146.5 (CH), 144.9 (Cq), 141.2 (CH), 137.1 (Cq), 137.0 (Cq), 136.7 (Cq), 136.5 (Cq), 119.3 (Cq), 125.8 (Cq), 132.7 (CH), 132.2 (CH), 129.2 (CH), 129.1 (2C, CH), 129.0 (CH), 128.6 (CH), 127.9 (CH), 126.4 (Cq), 120.7 (CH), 120.1 (CH), 119.7 (CH), 118.0 (Cq), 111.3 (Cq), 110.5 (CH), 106.4 (Cq), 68.7 (1C, CHisoprop) 51.7 (2C, CH2), 22.7, 22.3 (2C, CH3isoprop), 20.9, 18.9, 18.1 (6C, CH3mes 7, 7?, 8, 8?, 9?). (0104) Even if both of the catalysts possess two 5,7-dichloro-8-hydroxyquinolines, they show different NMR patterns. The different structures were revealed by X-ray diffraction. The crystals for the X-ray diffraction measurement were obtained by slow diffusion of Et2O in a saturated solution of CH2Cl2. The two derivatives exhibit a different geometry considering the 8-quinolinolate substituents. In derivative 3, the oxygen atoms of the two quinolinolates are orientated trans to each other, while in derivative 4 these trans positions are occupied by an oxygen and a nitrogen atom of the two different quinolinolates.

With the synthetic route has been constantly updated, we look forward to future research findings about (1,3-Dimesitylimidazolidin-2-ylidene)(2-isopropoxybenzylidene)ruthenium(VI) chloride,belong ruthenium-catalysts compound

Reference£º
Patent; Technische Universitaet Graz; Slugovc, Christian; Wappel, Julia; US8981024; (2015); B2;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

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.,50982-12-2

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%).

With the synthetic route has been constantly updated, we look forward to future research findings about Dichloro(cycloocta-1,5-diene)ruthenium(II),belong ruthenium-catalysts compound

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

As a common heterocyclic compound, it belong ruthenium-catalysts compound,Dichloro(cycloocta-1,5-diene)ruthenium(II),50982-12-2,Molecular formula: C8H12Cl2Ru,mainly used in chemical industry, its synthesis route is as follows.,50982-12-2

1,2-closo-C2B10H12 (0.400 g, 2.77 mmol) was dissolved in degassed THF (35 mL). Na metal (0.300 g, 13.04 mmol) and naphthalene (ca. 15 mg) were added and the solution stirred overnight. The resulting dark green solution was transferred via a gas-tight syringe into a second Schlenk tube containing [RuCl2(COD)]x (0.650 g, 2.32 mmol) and a large excess of naphthalene. The resulting brown mixture was heated at reflux for 90 min then allowed to cool to room temperature. The brown mixture was filtered through a short silica column eluting with DCM to afford a brown solution, removal of solvent from which yielded a brown solid. This was further purified by column chromatography (1:2 DCM:40-60 petroleum ether), giving a yellow band, followed by preparative TLC (4:3 DCM:40-60 petroleum ether, Rf 0.55) yielding, as major product C12H20B10Ru requires C 38.59, H 5.40. Found: C 38.01, H 5.67%.

With the synthetic route has been constantly updated, we look forward to future research findings about Dichloro(cycloocta-1,5-diene)ruthenium(II),belong ruthenium-catalysts compound

Reference£º
Article; Scott, Greig; Ellis, David; Rosair, Georgina M.; Welch, Alan J.; Journal of Organometallic Chemistry; vol. 721-722; (2012); p. 78 – 84;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

As a common heterocyclic compound, it belong ruthenium-catalysts compound,Dichloro(cycloocta-1,5-diene)ruthenium(II),50982-12-2,Molecular formula: C8H12Cl2Ru,mainly used in chemical industry, its synthesis route is as follows.,50982-12-2

[HNEt3][7,8-nido-C2B9H12] (0.400 g, 1.71 mmol) was suspended in degassed ether (35 mL). n-BuLi (1.40 mL, 3.50 mmol) was added, giving a pale yellow suspension which was stirred under N2 for 1 h, then heated at reflux for 90 min. The resulting solution was filtered, and the ether removed in vacuo to give a yellow oily solid which was subsequently dissolved in degassed THF (35 mL). [RuCl2(COD)]x (0.560 g, 2.00 mmol) and a large excess of naphthalene were added to the THF solution. The resulting brown mixture was heated at reflux for 90 min, then allowed to cool to room temperature. The brown mixture was filtered through a short silica column eluting with DCM to afford a brown solution, removal of solvent from which yielded a brown solid. This was further purified by column chromatography (1:2 DCM:40-60 petroleum ether) giving a yellow band, followed by preparative TLC (2:1 DCM:40-60 petroleum ether). C12H19B9Ru requires: C 39.85, H 5.30. Found: C 39.87, H 5.53%.

With the synthetic route has been constantly updated, we look forward to future research findings about Dichloro(cycloocta-1,5-diene)ruthenium(II),belong ruthenium-catalysts compound

Reference£º
Article; Scott, Greig; Ellis, David; Rosair, Georgina M.; Welch, Alan J.; Journal of Organometallic Chemistry; vol. 721-722; (2012); p. 78 – 84;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

As a common heterocyclic compound, it belong ruthenium-catalysts compound,Dichloro(cycloocta-1,5-diene)ruthenium(II),50982-12-2,Molecular formula: C8H12Cl2Ru,mainly used in chemical industry, its synthesis route is as follows.,50982-12-2

Complex C-l was also prepared using [RuCl2(COD)]n as a precursor. Thus, a mixture of [RuCl2(COD)]n (309 mg, 1.103 mmol), PPh3 (289 mg, 1.103 mmol) and ligand Id (248 mg, 1.103 mmol) was stirred in toluene (10 ml) at 115C for 24 h in a KONTES pressure tube. After cooling, the resulting brick colored precipitate was filtered on a filter frit, washed with diethyl ether (3 x 10 ml) and vacuum dried to afford 494 mg of a light pink crude material (Found C, 53.43; H, 5.26; N, 4.08%). Recrystallization from hot THF, filtering and layering with diethyl ether, afforded burgundy crystals (261 mg, 32% yield as a THF solvate). Based on NMR analysis, these crystals represent a THF solvate of complex C-l. The crystals were found to lose solvent based on elemental analysis. Elem. Anal: Calc’d for C3oH35Cl2N2PRuS (658.63): C, 54.71; H, 5.36; N, 4.25%; Found C, 54.37; H, 5.66; N, 3.87%.

With the synthetic route has been constantly updated, we look forward to future research findings about Dichloro(cycloocta-1,5-diene)ruthenium(II),belong ruthenium-catalysts compound

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

Dichloro[1,3-bis(2,4,6-trimethylphenyl)-2-imidazolidinylidene][[5-[(dimethylamino)sulfonyl]-2-(1-methylethoxy-O)phenyl]methylene-C]ruthenium(II), cas is 918870-76-5, it is a common heterocyclic compound, the ruthenium-catalysts compound, its synthesis route is as follows.,918870-76-5

Example 103 Synthesis of Ru complex 6h The Ru complex (Zhan catalyst 2b, l.Ommol) and a new ligand 5h (1.5mmol) were dissolved in 20 mL of anhydrous DCM and reacted directly to form the desired Ru complex 6h in the preaence of CuCl (3.0mmol) in a 100 mL of three-neck flask filled with inert gas (Ar). The reaction mixture was stirred for 0.5 hr at room temperature. After complete, the reaction solution was filtered and purified by flask column. 378mg of yellow-green solid product 6h was obtained, yield: 52%. Ru complex 6h is confirmed by 1HNMR (400 MHz, CDC13): delta 16.52 (s, 1H, Ru=CH), 8.43 (s, 1H, N=CH), 8.10 (s, 1H), 7.46-7.22 (m, 2H), 7.73-6.96 (m, 8H), 4.19 (s, 4H, NCH2CH2N), 3.95 (s, 3H), 3.87 (s, 3H), 2.49 (s, 12H), 2.48 (s, 6H).

With the synthetic route has been constantly updated, we look forward to future research findings about Dichloro[1,3-bis(2,4,6-trimethylphenyl)-2-imidazolidinylidene][[5-[(dimethylamino)sulfonyl]-2-(1-methylethoxy-O)phenyl]methylene-C]ruthenium(II),belong ruthenium-catalysts compound

Reference£º
Patent; ZANNAN SCITECH CO., LTD.; ZHAN, James Zheng-Yun; WO2011/79439; (2011); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI