Day: August 26, 2020

Benzylidenebis(tricyclohexylphosphine)dichlororuthenium, cas is 172222-30-9, it is a common heterocyclic compound, the ruthenium-catalysts compound, its synthesis route is as follows.

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).

As the rapid development of chemical substances, we look forward to future research findings about 172222-30-9

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

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.

The catalyst precursor, preferably [RuCI2(COD)]m (1 eq.) (COD = cis,cis-cycloocta-1 ,5 diene), 1 ,4-bis(diphenylphosphino)butane (1.0-1 .2 eq., preferably 1.0 eq.) and 2-picolylamine (1 .0-1.4 eq., preferably 1.225 eq.) were dissolved in one of the above mentioned solvents, preferably methyl isobutylketone (10-20 ml/g Ru-precursor, preferably 20 ml/g). The mixture was heated to reflux for 3 – 5 hours and then cooled to ambient temperature. The solid precipitate was filtered off and washed with the same solvent that was used for the reaction. A person skilled in the art can determine the cis-/trans- isomeric ratio by NMR. The diastereomeric ratios generated by this method are usually in the range of d.r. (diastereomeric ratio) >98% towards the cis isomer. The same results can be achieved starting with [RuCI2(dmso-KS)3(dmso-KO)], [RuCI2(dmso-KS)4]or [RuCI2(bicyclo[2.2.1 ]hepta- 2,5-diene)]m as precursor

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

Reference£º
Patent; SYNGENTA PARTICIPATIONS AG; LOTHSCHUETZ, Christian; SAINT-DIZIER, Alexandre Christian; WO2014/166777; (2014); 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.

The catalyst precursor, preferably [RuCI2(COD)]m (1 eq.), 1 ,4-bis(diphenylphosphino)butane (1 .0-1 .2 eq., preferably 1 .0 eq.) and 2- quinolinylmethylamine (1.0-1 .4 eq., preferably 1.225 eq.) were dissolved in one of the above mentioned solvents, preferably cyclohexanone (10- 20 ml/g Ru-precursor, preferably 20 ml/g). The mixture was heated at 130 C for 1 hour and then cooled to ambient temperature. The solid precipitate was filtered off and washed with the same solvent that was used for the reaction. A person skilled in the art can determine the cis-/trans- isomeric ratio by NMR. The diastereomeric ratios generated by this method are usually in the range of d.r. (diastereomeric ratio) >98% towards the cis isomer. The same results can be achieved starting with [RuCI2(dmso-KS)3(dmso-KO)], [RuCI2(dmso-KS)4]or [RuCI2(bicyclo[2.2.1]hepta-2,5-diene)]m as precursor

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

Reference£º
Patent; SYNGENTA PARTICIPATIONS AG; LOTHSCHUETZ, Christian; SAINT-DIZIER, Alexandre Christian; WO2014/166777; (2014); 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.

11 g of trimethylsilyl chloride was dissolved in 30 mol of well dried tetrahydrofuran in a 300 ml flask whose inside had been substituted by nitrogen, and the obtained solution was cooled to -78 C. 100 ml of a tetrahydrofuran solution (2.0 mol/l) of cyclopentadienyl sodium was added dropwise to the above solution in a stream of nitrogen over 1 hour. The solution was stirred at -78 C. for 1 hour and returned to room temperature over 6 hours. A salt precipitated in the mixture solution was removed by filtration in a nitrogen atmosphere, and the residual solution was distilled to obtain 8 g of trimethylsilyl cyclopentadiene. 0.5 g of metal sodium was mixed with a well dried tetrahydrofuran solution in a 300 ml flask whose inside had been substituted by nitrogen, and the resulting solution was cooled to -78 C. A solution of 2.5 g of the above synthesized trimethylsilyl cyclopentadiene dissolved in 30 ml of tetrahydrofuran was added dropwise to the above solution in a stream of nitrogen over 1 hour and further heated to room temperature under agitation for 3 hours to obtain a tetrahydrofuran solution of trimethylsilyl cyclopentadienyl sodium. Separately, 5 g of dichloro(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 synthesized tetrahydrofuran solution of trimethylsilyl cyclopentadienyl sodium was added dropwise to the above solution in a stream of nitrogen over 1 hour. The resulting solution was stirred at -78 C. for 3 hours and returned to room temperature under agitation over 12 hours. After the 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 0.9 g of bis(trimethylsilylcyclopentadienyl)ruthenium (yield rate of 13%).

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

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

172222-30-9, Benzylidenebis(tricyclohexylphosphine)dichlororuthenium is a ruthenium-catalysts compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

EXAMPLE 1 Metathesis by Ethenolysis of Methyl Oleate Catalyzed by a Type 3 Complex (FIG. 1) in an Ionic Liquid; 1 ml of 3-butyl-1,2-dimethylimidazolium bis-triflylamide with formula [BMMI]+[N(CF3SO2)2]- pre-dried overnight at 80 C., 148 mg of methyl oleate (source: Fluka, with a purity higher than 98%) and 15 mg of the complex with formula Cl2Ru(CH-o-O-iPrC6H4)PCy3 (synthesized by reacting the 1st generation Grubbs complex with formula Cl2Ru(CHC6H5)(PCy3)2 with 1-isopropoxy-2-vinylbenzene in the presence of CuCl), this corresponding to 5% molar of catalyst with respect to methyl oleate, were introduced, in an inert atmosphere of argon, into an autoclave reactor provided with an agitation system and a pressure sensor. The autoclave was then placed under vacuum and pressurized to obtain a pressure of 10 bars (1 MPa) of ethylene (origin: Alphagas, quality N25). The temperature was kept constant at 20 C. The medium was stirred at ambient temperature for 2 hours, then the excess ethylene was slowly purged by returning to atmosphere pressure at a temperature not exceeding 20 C. and the autoclave was again placed under an atmosphere of argon. The products were separated from the ionic liquid by adding 2 to 3 ml of heptane distilled over CaH2 and degassed. An aliquot (100 mul) of the extracted solution was passed through a short silica column (2 cm) eluted with diethyl ether. It was analyzed by gas phase chromatography (ZB-1 column, 100% dimethylpolysiloxane, 30 metres, helium vector gas 2 ml/min, temperature programming: 60 C. then 5 C./min to 220 C.) coupled to a mass spectrometer. The methyl oleate conversion was 95%. It was calculated using decane as an internal reference. The reaction products were composed of 1-decene (fraction A) and methyl decenoate (fraction B). The presence of 1-decene isomers was not detected. Homo-metathesis products were present in trace amounts and could not be quantified.

The synthetic route of 172222-30-9 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Olivier-Bourbigou, Helene; Vallee, Christophe; Hillion, Gerard; US2007/179307; (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.

In a glove box, NHC ligand precursor 23 (63 mg, .13, mmol), ruthenium precursor 11 (78 mg, .13 mmol) and KOMJu(Fe) (29 mg, .13 mmol) were combined in toluene. The flask was sealed, removed from the glove box and stirred at 60 0C for 18 hours. The reaction was concentrated and purified by flash column chromatography (5% –> 20% Et2O/Pent). There were 3 bands that could be isolated from this column, first 2 brown bands and then one green band. The second brown band was the desired product; however, it was not completely pure after one column. Recolumning in 10% Et2O/Pentane gave a brown oil product completely pure by 1H NMR (9 mg, 9%) and another fraction still slightly impure (18 mg, 18%). The products were lyophilized from benzene to give solids. 1H NMR (300 MHz, CDCl3) delta 16.78 (s, IH), 8.13 (br, 2H), 7.74-7.62 (m, 4H), 7.07-7.04 (m, IH), 6.97 (dd, J = 3, 1.5 Hz, IH), 6.66 (t, J = 7.5 Hz, 3H), 6.34 (d, J = 8.4 Hz, IH), 4.49 (sept, J = 6 Hz, IH), 1..44 (d, J = 6 Hz, 6H), 1.44 (br, 18H), 1.18 (br, 18H); 13C (75 MHz, CDCl3) delta; HRMS (EI+) calc for C4IH56Cl2N2ORu, 764.2814. Found 764.2842.

As the paragraph descriping shows that 203714-71-0 is playing an increasingly important role.

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.20759-14-2,Ruthenium(III) chloride hydrate,as a common compound, the synthetic route is as follows.

(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).

As the paragraph descriping shows that 20759-14-2 is playing an increasingly important role.

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

172222-30-9, Benzylidenebis(tricyclohexylphosphine)dichlororuthenium is a ruthenium-catalysts compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

In a dry box, a Teflon-sealed n.m.r. tube was charged with (2S)-methyl 2-N-acetylaminopenta-2,4-dienoate 57 (10.8 mg, 63.9 mumol), Grubbs’ catalyst (50.7 mg, 61.6 mumol) and degassed deuterated DCM (CD2Cl2, 0.8 mL) at room temperature. The n.m.r. tube was shaken gently and reaction progress was monitored by 1H and 31P n.m.r. spectroscopy. Compounds were identified by the following diagnostic resonances: 1H n.m.r. (300 MHz, CD2Cl2): After 15 min: Grubbs’ catalyst: delta 8.61 (d, J=7.6 Hz, 2H, ortho-Arom CH), 20.05 (s, 1H, [Ru]CHPh); Ruthenium-dienamide complex 73: delta 7.96 (d, J=11.0 Hz, 1H, [Ru]CHCH), 20.11 (d, J=11.0 Hz, 1H, [Ru]CH); Ruthenium-dienamide chelate 74 (trace): delta 15.20 (d, J=4.2 Hz, 1H, [Ru]CH); Ratio of ruthenium complexes [Ru]CHPh: 73: 74=1.0:1.0:<0.1. After 60 min: Grubbs' catalyst: delta 8.45 (d, J=7.6 Hz, 2H, ortho-Arom CH), 20.04 (s, 1H, [Ru]CHPh); Ruthenium-dienamide complex 73: delta 7.96 (d, J=11.0 Hz, 1H, [Ru]CH=CH), 20.10 (d, J=11.0 Hz, 1H, [Ru]CH); Ruthenium-dienamide chelate 74: delta 6.73 (d, J=3.0 Hz, 1H, [Ru]CHCH), 15.19 (d, J=4.2 Hz, 1H, [Ru]CH); Ratio of ruthenium complexes [Ru]CHPh: 73: 74=3:1:1. After 120 min (no change after 18 h): Ruthenium-dienamide chelate 74: delta 6.71 (d, J=3.0 Hz, 1H, [Ru]CHCH), 15.19 (d, J=4.0 Hz, 1H, [Ru]CH). 31P n.m.r. (300 MHz, CDCl3): delta Ruthenium-dienamide chelate 74: 35.0; Grubbs' catalyst: 37.0; Ruthenium-dienamide complex 73: 38.8; Tricyclohexylphosphine oxide: 46.5. The synthetic route of 172222-30-9 has been constantly updated, and we look forward to future research findings. Reference£º
Patent; Robinson, Andrea; Elaridi, Jomana; US2007/197429; (2007); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

203714-71-0, Dichloro(2-isopropoxyphenylmethylene)(tricyclohexylphosphine)ruthenium (II) is a ruthenium-catalysts compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

PIB-supported Grubbs-Hoveyda 2nd generation catalyst (molecule 8): A mixture of 1.14 g (0.48 mmol) of 1,3-bis(2,6-dimethyl-4-(polyisobutyl)phenyl)-4,5-dihydro-imidazolium tetrafluoroborate, 0.15 g (0.75 mmol) of KHMDS, 0.05 g (0.5 mmol) of CuCl and 0.36 g (0.57 mmol) of 1st generation Hoveyda-Grubbs catalyst was prepared was dissolved in 5 mL of toluene. The solution was heated to 100 C. for 3 hours. Solvent was removed under reduced pressure and purified by column chromatography (dichloromethane) resulting in a dark green viscous residue. The yield was 60% (0.75 g). 1H-NMR (500 MHz, CDCl3), delta: 0.8-1.6 (m, 280H), 1.87 (s, 2H), 2.41 (b, 6H), 2.62 (b, 6H) 4.15 (s, 4H), 4.90 (m, 1H) 6.8 (m, 2H), 6.98 (m, 1H), 7.22 (b, 4H), 7.47 (m, 1H), and 16.67 (s, 1H). 13C NMR (125 MHz, CDCl3), delta: 21.62, multiple peaks between 30-40 and 58-60, 113.10, 122.42, 123.09, 126.53, 127.01, 129.69, 137.30, 139.21, 145.41, 145.44, 152.16, 152.43, 152.45, 211.19, and 297.23 (m).

As the paragraph descriping shows that 203714-71-0 is playing an increasingly important role.

Reference£º
Patent; Bergbreiter, David E.; Bazzi, Hassan S.; Hongfa, Chayanant; US2009/203860; (2009); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI