Day: September 3, 2020

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.172222-30-9,Benzylidenebis(tricyclohexylphosphine)dichlororuthenium,as a common compound, the synthetic route is as follows.,172222-30-9

In a glove box, NHC ligand precursor 23 (162 mg, .34 mmol), ruthenium precursor 5 (150 mg, .27 mmol) and KOt-Bu(Fe) (74 mg, .34 mmol) were combined in C6D6 and stirred at RT for 2.5 hours. The flask was sealed, removed from the glove box and the reaction was concentrated and purified by flash column chromatography (2.5percent – > 5percent Et2psi/Pent) to yield a brown oil. The brown oil was lyophilized from benzene to give 25 as a brown solid (66 mg, 25percent). 1H NMR (300 MHz3 CDCl3) delta 20.07 (d, J = 10.5 Hz, IH)3 8.03 (br, 2H), 7.60 (t, 1.8 Hz, IH), 6.86-6.81 (ra, 2H), 6.51 – 6.47 (m, IH), 1.81 – 1.07 (m).

172222-30-9 Benzylidenebis(tricyclohexylphosphine)dichlororuthenium 60145889, aruthenium-catalysts compound, is more and more widely used in various.

Reference£º
Patent; MATERIA, INC.; CALIFORNIA INSTITUTE OF TECHNOLOGY; WO2007/75427; (2007); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.203714-71-0,Dichloro(2-isopropoxyphenylmethylene)(tricyclohexylphosphine)ruthenium (II),as a common compound, the synthetic route is as follows.,203714-71-0

A dry, 1000-mL, one-necked, round-bottomed flask is equipped with a magnetic stirring bar, rubber septum and an argon inlet. The flask is charged under an argon atmosphere with a solid SIMES x HBF4 2 (35.28 mmol, 13.9 g) and dry n-hexane (400 ml_). A solution of potassium tert-amylate (21.6 ml_, 36.75 mmol) is added from a syringe and the resulting mixture is stirred under argon at room temperature for 1 h. To the resulted solution a solid Hoveyda-Grubbs 1st generation catalyst 1 (29.4 mmol, 17.6 g) is added in one portion. The flask is equipped with a reflux condenser with an argon inlet at the top and the reaction mixture is refluxed for 2 h. The contents of the flask are cooled to room temperature and solid CuCI (51.45 mmol, 5.1 g) is added slowly in three portions and the resulting mixture is refluxed for 2 h. From this point forth, all manipulations are carried out in air.; 1.11. Isolation of the product by crystallization; The reaction mixture is evaporated to dryness and re-dissolved in ethyl acetate (200 ml_). The solution is filtrated through a Buchner funnel with glass frit filled with Celite and then concentrated in vacuo. The residue is dissolved in ambient temp. 1 :10 v/v mixture of CH2CI2 and methanol (220 ml_). After concentration to ca. % of the initial volume using a rotary evaporator (room temperature) crystals are precipitated. These crystals are filtered- off on a Buchner funnel with glass frit. The crystals are washed twice with small portions of CH3OH (-20 ml_), and dried in vacuo to give pure Hoveyda 2nd catalysts 3 (25.3 mmol, 15.81 g). The filtrate after crystallization is evaporated to dryness and crystallized for the second time from CH2CI2 and methanol using the same protocol giving an additional crop of pure Hoveyda 2nd generation catalyst (1.7 mmol, 1.08 g). The total yield of pure Hoveyda-Grubbs 2nd generation catalyst 3 is 92% (27.0 mmol, 16.9 g).

203714-71-0 Dichloro(2-isopropoxyphenylmethylene)(tricyclohexylphosphine)ruthenium (II) 10941020, aruthenium-catalysts compound, is more and more widely used in various.

Reference£º
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; BOEHRINGER INGELHEIM PHARMA GMBH & CO. KG; WO2007/54483; (2007); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

As a common heterocyclic compound, it belongs to ruthenium-catalysts compound, name is (1,3-Dimesitylimidazolidin-2-ylidene)(2-isopropoxybenzylidene)ruthenium(VI) chloride, and cas is 301224-40-8, its synthesis route is as follows.

301224-40-8, cis-RuC12(slMes)( CHC6H4O1-Pr)(PhP(OMe)2), cis-C797: To a round-bottomed flask was charged C627 (15.0 g), degassed CH2C12 (1000 mL) and a magnetic stir bar under nitrogen, followed the addition of phosphonite PhP(OMe)2 (4.1 g). The solution was stirred for 3.7 h and second portion of phosphonite PhP(OMe)2 (2.05 g) was added. The solution was continued to stir for 2 more hours and the solution was concentrated by a rotary evaporator. A silica gel plug column (4 x 2.5 in, D x H) was pre-wetted with CH2C12. Low vacuum suction was used to assist elution. The crude was loaded on the top of the column. The first eluent was CH2C12 and a green fraction was collected, that was C627 as verified by NIVIR. The green fraction was followed by a yellow fraction that appeared to be an oxidation derivative of the phosphonite. The eluent was then switched to gradient mixture of CH2C12 /EtOAc. A brown band containing the product was collected. The solvent was removed by a rotary evaporator and the residue was recrystallized from CH2C12 /heptanes. black crystalline solid was obtained (3.1 g). ?H NMR (400 IVIHz, CD2C12, ppm): oe 15.83 (d, J = 24 Hz, 1H, Ru=CI]), 9.16 (dd, J = 8 Hz, J = 2 Hz, 1H), 7.51 (m, 1H), 7.25 (m, 1H), 7.15 (m, 2H), 7.02 – 6.88 (m, 5H), 6.66 (s, 1H), 6.61 (d, J = 8 Hz, 1H), 6.14 (s, 1H), 4.49 (septet, J = 6Hz, 1H, CIJMe2), 4.02-3.62 (m, 4H, CH2CH2), 3.33 (d, J = 11 Hz, 3H, OCH3), 3.05 (d, J = 12 Hz, OCH3), 2.67 (s, 3H, mestyl methyl), 2.62 (s, 3H, mestyl methyl), 2.46 (s, 3H, mestyl methyl), 2.33 (s, 3H, mestyl methyl), 2.22 (s, 3H, mestyl methyl), 1.95 (s, 3H, mestyl methyl), 1.46 (d, J = 6Hz, 3H, CH(CH3)2), 1.19 (d, J = 6Hz, 3H, CH(CH3)2).3?P NIVIR (161.8 IVIFIz, CD2C12, ppm): oe 163.84 (b).

With the complex challenges of chemical substances, we look forward to future research findings about 301224-40-8,belong ruthenium-catalysts compound

Reference£º
Patent; MATERIA, INC.; GIARDELLO, Michael, A.; TRIMMER, Mark, S.; WANG, Li-Sheng; DUFFY, Noah, H.; JOHNS, Adam, M.; RODAK, Nicholas, J.; FIAMENGO, Bryan, A.; PHILLIPS, John, H.; (127 pag.)WO2017/53690; (2017); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

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

Na2[7,10-nido-C2B10H12] was dissolved in degassed THF (45 mL) giving a purple solution. Excess Na was removed from the reduced carborane solution to give a colourless solution which was then transferred into a Schlenk tube containing [RuCl2(COD)]x (0.780 g, 2.78 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 (2:1 DCM:40-60 petroleum ether, Rf 0.38) yielding solid. C12H20B10Ru requires C 38.59, H 5.40. Found: C 39.48, H 4.87%.

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

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 belongs to ruthenium-catalysts compound, name is (1,3-Dimesitylimidazolidin-2-ylidene)(2-isopropoxybenzylidene)ruthenium(VI) chloride, and cas is 301224-40-8, its synthesis route is as follows.,301224-40-8

Hoveyda-Grubbs second generation catalyst H2 (104 mg, 0.16 mmol) and potassium 2,6-dimethylbenzenethiolate (34 mg, 0.19 mmol) 2b were transferred to a 25 mL Schlenk flask, followed by addition of 4 mL of toluene and 1 mL THF under argon. Then the mixture was stirred vigorously at 20 C. for 30 min. During this time the color of the mixture turned from light green to a slightly darker green. The reaction mixture was filtered, and the volume of the filtrate reduced to about 3 mL. Hexane (15 mL) was added to the filtrate to precipitate the product 4b as red/orange-brown micro-crystals (86.3 mg, 71%). (0121) Crystals for X-ray diffraction analysis (see FIG. 12 and Table 4) were prepared by dissolving a sample in a minimal amount of toluene, upon which a layer of hexane was added. Red-brown crystals were formed over a period of 3 days at room temperature. (0122) 1H NMR (400.13 MHz, CDCl3): delta=14.90 (s, 1H), 7.22 (m, 1H), 7.10 (s, 2H), 7.06 (s, 2H), 6.80-6.73 (m, 2H), 6.66 (t, J=7.2 Hz, 1H), 6.16 (d, J=8.0 Hz, 1H), 4.15 (m, 4H), 3.83 (sep, J=6.16 Hz, 1H), 2.62 (s, 6H), 2.54 (s, 6H), 2.42 (s, 6H), 2.32 (br s, 3H), 1.8 (d, J=5.6 Hz, 3H), 0.89 (d, J=6.4 Hz, 3H), 0.80 (br s, 3H). 13C NMR (100.6 MHz, CDCl3): delta=271.29, 211.87, 151.57, 145.12, 142.30 (br), 141.67, 139.25, 138.90, 138.75, 137.40 (br), 129.74, 129.43, 127.32, 126.61, 124.43, 123.12, 122.34, 114.19, 74.99, 52.15, 21.55, 21.45, 21.43, 20.07 (br). (0123) A corresponding ORTEP-style diagram of 4b is shown in FIG. 12. Selected geometrical parameters: Ru1-C9=1.846 , Ru1-S1=2.285 , Ru1-Cl1=2.364 , Ru1-O1=2.298 , Ru1-S1-C1=113.67, Cl1-Ru1-S1=150.75.

With the complex challenges of chemical substances, we look forward to future research findings about (1,3-Dimesitylimidazolidin-2-ylidene)(2-isopropoxybenzylidene)ruthenium(VI) chloride

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

It is a common heterocyclic compound, the ruthenium-catalysts compound, Ruthenium(III) chloride hydrate, cas is 20759-14-2 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 complex challenges of chemical substances, we look forward to future research findings about Ruthenium(III) chloride hydrate

Reference£º
Patent; Banyu Pharmaceutical Co., Ltd.; US6326375; (2001); B1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Name is Ruthenium(III) chloride, as a common heterocyclic compound, it belongs to ruthenium-catalysts compound, and cas is 10049-08-8, its synthesis route is as follows.,10049-08-8

[(1S,3R)-1-(Methoxycarbonylamino-methyl)-3-methyl-cyclopentyl]-acetic acid ((1S,3R)-1-Benzyl-3-methyl-cyclopentylmethyl)-carbamic acid methyl ester (2.6 g, 9.9 mmol) and sodium periodate (29.8 g, 140 mmol) were stirred together in carbon tetrachloride (30 mL), acetonitrile (30 mL), and water for 6 hours. The mixture was cooled to 0¡ã C., and ruthenium(III) chloride (0.04 g, 0.2 mmol) was added to the reaction mixture. The reaction was allowed to warm to room temperature and stirred for 20 hours. Diethyl ether (50 mL) was added, and the mixture was then extracted with saturated aqueous sodium hydrogen carbonate (200 mL). The aqueous layer was acidified to pH 1 with 4N hydrochloric acid and re-extracted with ethyl acetate (200 mL), dried (MgSO4), and the solvent was evaporated under reduced pressure. The residue was purified by chromatography (silica gel, eluding with a gradient of heptane to 1:1 heptane:ethyl acetate) to give 0.32 g (14percent) of [(1S,3R)-1-(methoxycarbonylamino-methyl)-3-methyl-cyclopentyl]-acetic acid; Rf (heptane-ethyl acetate, 8:2) 0.30; IR thin film (cm-1) 3338 (NH), 1712 (C=O); 1H-NMR (400 MHz; CDCl3): delta 9.29 (1H, s, COOH), 5.17 (1H, bs, NH), 3.71 (3H, s, OMe), 3.30 (1H, dd, J 14.4, 7.1, CHAHBNH2), 3.17 (1H, dd, J 14.4, 6.6, CHAHBNH2), 2.37 (2H, s, CH2COOH), 2.20-1.00 (7H, m), 1.01 (3H, d, J 6.4, CHMe); MS (ES+) m/z 230 (M+H, 63percent), 481 (M+Na,100).

With the complex challenges of chemical substances, we look forward to future research findings about Ruthenium(III) chloride

Reference£º
Patent; Bryans, Justin Stephen; Blakemore, David Clive; Williams, Sophie Caroline; US2003/69438; (2003); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

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

A mixture of [RuCl2(COD)]n (155 mg, 0.552 mmol) and la (147 mg, 0.552 mmol) was stirred in toluene (10 ml) at 115 C for 48 h in Kontes pressure tube. After cooling, a brick-colored precipitate was collected on a filter frit, washed with Et20 (3 x 10 ml) and vacuum dried on the filter. The material was extracted on the filter with 5 x 3 ml CH2C12 allowing the filtrates to be collected in 5 separate vials. A red solution in each vial was layered with Et20 (20 ml). In 1 week, the combined precipitates (or red crystals) from each vial were collected, washed with Et20 (3 x 10 ml) and vacuum-dried to afford 144 mg of the desired product (60%). Elem. Anal: Calcd for C28H44CI4N4O2RU2S2 (876.75): C, 38.36; H, 5.06; N, 6.39%. Found C, 38.38; H, 4.99; N, 6.32%. Elem. Anal: Calcd for C28H44CI4N4O2RU2S2 (876.75): C, 38.36; H, 5.06; N, 6.39%. Found (under nitrogen): C, 38.61; H, 4.99; N, 6.17%. The complex is poorly soluble in CDC13, slightly better in CD2C12. 1H NMR (400 MHz, CD2C12, r.t., saturated): delta 2.00 (brs, 1H), 2.15 (d, J~ 14 Hz, 1H), 2.37 (t, J~ 12 Hz, 1H), 2.15 (m, 4H), 2.75-2.94 (m, 3H), 3.04 (d, J~ 14 Hz, 1H), 3.07-3.23 (m, 5H), 3.38 (m, 2H), 3.44-3.62 (m, 3H), 3.61-3.75 (m, 3H), 3.79 (d, J~ 12 Hz, 1H), 3.87 (t, J~ 14 Hz, 1H), 3.93-4.09 (overlapped m, 3H), 4.06 (brs, 1H), 4.44 (t, J~ 11 Hz, 1H), 4.72 (brs, 1H, possibly NH), 5.07 (d, J~ 18 Hz, 1H), 6.72-8.85 (overlapped, 10H), 9.19 (brs, 1H, NH – C1). The same compound is obtained if the synthesis is carried out in the presence of P(C6F5)3. (0457) [0216] An X-ray structure of complex K-1 revealed that one ligand coordinates to one Ru atom via mer-fashion. A second ligand coordinates to second Ru atom via ^ac-fashion. Both Ru atoms are connected via one bridging CI atom. One S(Ph) atom is part of mer-coordinated la. There appears to be a hydrogen-bonding interaction between one NH group of the fac- coordinated ligand and terminal CI atom attached to the first Ru atom. Complex K-1 exists as a single species in solution. The NH hydrogen atom H-bonded to the chloride ligand appears at delta 9.19 ppm in the 1H NMR spectrum. It is shifted to low field by Deltadelta = 4.47 ppm relative to the NH resonance of the non-H bonded NH group.

With the complex challenges 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

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

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.

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

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

Name is Dichloro(2-isopropoxyphenylmethylene)(tricyclohexylphosphine)ruthenium (II), as a common heterocyclic compound, it belongs to ruthenium-catalysts compound, and cas is 203714-71-0, its synthesis route is as follows.,203714-71-0

NHC ligand precursor 10 (156 mg, .3 mmol), KOz-Bu(F g) (66 mg, .3 mmol), and ruthenium complex 11 (132 mg, .22 mmol) were all combined in toluene in a glove box. The flask was removed and stirred at 60 0C for 18 hours in a fume hood. The reaction mixture was then directly purified by flash column chromatography (5% Et2theta/Hexanes, run 2 times) to yield catalyst 12 (34 mg, 20%) as a green oil. The catalyst was then lyophilized from benzene to give a pale green solid. It should be noted that by 1H NMR the conversion to 12 is 50%. 1H NMR (300 MHz, CDCl3) delta 16.91 (IH, s), 8.14-8.13 (2H, m), 7.73 (2H, m), 7.64 (IH, m), 7.52 (IH, m), 7.06-6.92 (2H, m), 6.62 (IH, t, J = 7.5 Hz), 6.31 (IH, d, J – 8.4 Hz), 4.47 (IH, quint, J = 6 Hz), 3.51 (4H, s), 1.51 (18H, s), 1.35 (6H, d, J = 6 Hz), 1.24 (18H, s); HRMS (EI+) calc for C4IH58N2OCl2Ru 766.2970. Found 766.3007. Fig. 4 depicts the single crystal X-ray structure was obtained for catalyst 12.

With the complex challenges of chemical substances, we look forward to future research findings about Dichloro(2-isopropoxyphenylmethylene)(tricyclohexylphosphine)ruthenium (II)

Reference£º
Patent; MATERIA, INC.; CALIFORNIA INSTITUTE OF TECHNOLOGY; WO2007/75427; (2007); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI