Day: September 29, 2020

Dichlorotris(triphenylphosphino)ruthenium (II), cas is 15529-49-4, it is a common heterocyclic compound, the ruthenium-catalysts compound, its synthesis route is as follows.,15529-49-4

Compound 5 (300.0 mg, 0.68 mmol) and degassed morpholine (10 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 thin-layer chromatography (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. After sufficiently removing the morpholine, dichlorotris(triphenylphosphino)ruthenium (II) (648.6 mg, 0.68 mmol) and dehydrated toluene (15 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 two hours, and the reaction mixture was restored to room temperature (25 C.). 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 an hour, the generated purple substance was filtered out in an argon atmosphere while being washed with dehydrated diethylether, thereby obtaining a crude product. Subsequently, the resulting crude product was subjected to column chromatography (developing solvent: chloroform/ethyl acetate=5/1) in which silica gels are 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 204.3 mg (0.35 mmol, 51%)of substantially pure Compound 2b (RUPIP2) as a purple substance. The spectral data of Compound 2b (RUPIP2) is shown below. 1H NMR (600 MHz, CDCl3): delta 7.89 (d, 2H, J=8.3 Hz, C10H6N2), 7.69 (t, 2H, J=7.6 Hz, C10H6N2), 7.59 (d, 2H, J=8.3 Hz, C10H6N2), 3.89 (d, 4H, J=7.6 Hz, PCH2), 2.67-2.78 (m, 4H, CH(CH3)2), 1.35-1.43 (m, 24H, CH(CH3)2). 13C NMR (151 MHz, CDCl3): delta 163.3, 158.3, 134.4, 121.9, 120.0, 42.1 (d, 1JPC=20.2 Hz), 25.4, 20.5, 19.4. 31P{1H} NMR (243 MHz, CDCl3): delta 60.6. HRMS (ESI, (M-Cl)+) Calcd for C24H38ClN2P2Ru+: 553.1242. Found m/z=553.1240.

With the rapid development of chemical substances, we look forward to future research findings about Dichlorotris(triphenylphosphino)ruthenium (II)

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

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.246047-72-3,(1,3-Bis(2,4,6-trimethylphenyl)-2-imidazolidinylidene)dichloro(phenylmethylene)(tricyclohexylphosphine)ruthenium,as a common compound, the synthetic route is as follows.

After a 50 mL two-necked flask was purged with argon, the ligand 3cw (10 mmol), CuCl (30 mmol, 3 eq) and 30 mL of dry DCM were sequentially added and the mixture was purged three times with argon to protect the closed system with an argon balloon. Ruthenium complex 1b (12 mmol) was added under argon atmosphere, and the reaction was carried out at room temperature for 0.5 hour. After the reaction was over, silica gel was added to the filtrate after filtration to obtain sand. The crude product was obtained by silica gel column chromatography and then washed with methanol or pentane-DCM to obtain a green solid product 4cw, yield: 85%.

246047-72-3, As the paragraph descriping shows that 246047-72-3 is playing an increasingly important role.

Reference£º
Patent; Zannan Science And Technology (Shanghai) Co., Ltd.; Zhan Zhengyun; (102 pag.)CN104262403; (2017); B;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

246047-72-3, (1,3-Bis(2,4,6-trimethylphenyl)-2-imidazolidinylidene)dichloro(phenylmethylene)(tricyclohexylphosphine)ruthenium is a ruthenium-catalysts compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example 1Synthesis of Ru complex 4a (H2IMes)(PCy3)Cl2Ru=CHPh (formula lb, 860mg, l .Ommol) and CuCl (270 mg, 2.5mmol, 2.5 eq) were added into a 100 mL of two-neck round-bottom flask filled with inert gas (Ar), and followed by adding DCM (15 mL) and ligand 3a (250 mg, 1.2mmol, 1.2 eq) into the DCM solution at 20-25C. The reaction was stirred until completed in 30-60 min. (monitored by TLC). The reaction mixture was filtered and concentrated, then purified by flash column eluting with a gradient solvent (Pentane/DCM 2/1 to DCM). The purified solid product was washed with methanol, and dried under vacuum to obtain 27mg of green solid product 4a, yield: 4%. The green product was confirmed by 1HNMR. Ru complex (4a) 1HNMR (400 MHz, CDC13): delta 19.09 (s, lH, Ru=CH),7.51-6.70 (m, 13H), 5.31 (m, 1H), 4.30 (d, J = 12.9 Hz, 1H), 4.04 (s, 4H, NCH2CH2N), 3.61 (d, J= 12.9 Hz, 1H), 2.45 (s, 12H), 2.33 (s, 6H).; Example 9 Synthesis of Ru complex 4j The synthetic procedure is the same as in Example 1 in 1.0 mmol scale. 353 mg of green solid product 4j was obtained (yield: 48%). Ru complex (4j) 1H- MR (400 MHz, CDC13): delta 18.88 (s, lH, Ru=CH), 7.57-6.44 (m, 11H), 5.36 (t, J = 13.2 Hz, 1H), 4.16-4.02 (m, 5H), 4.01 (d, J = 13.2 Hz, 1H), 2.75-2.00 (m, 19H), 1.01-0.90 (m, 6H)., 246047-72-3

As the paragraph descriping shows that 246047-72-3 is playing an increasingly important role.

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

Dichlorotris(triphenylphosphino)ruthenium (II), cas is 15529-49-4, it is a common heterocyclic compound, the ruthenium-catalysts compound, its synthesis route is as follows.,15529-49-4

Example 8: Dichloro[(N-(2-(diphenylphosphino)benzyl)-2-(ethylthio)ethanamine)(triphenylphosphine)]ruthenium(ll) 8 (8) Under argon 2-(methylthio)benzaldehyde (0.33 g, 2.18 mmol) is added to a solution of 2- (di-phenylphosphino)ethanamine (0.50 g, 2.18 mmol) in methanol (6 ml). After stirring for 42 h at 75 C the reaction mixture is cooled to room temperature and evaporated under vacuo. SNP-ligand 2-(diphenylphosphino)-N-(2-(methylthio)benzylidene)ethanamine is obtained as a light-brown solid (0.66 g, 84%). Analytical data: 1H-NMR (500 MHz, CDCl3): 8.74 (s, 1H), 7.79 (dd, 7=1.58, 7.88, 1H), 7.52-7.48 (m, 4H), 7.39- 5 7.32 (m, 8H), 7.21 (m, 1H), 3.80 (m, 2H), 2.53 (m, 2H), 2.48 (s, 3H). 13C-NMR (500 MHz, CDCl3): 159.37, 138.34, 134.24, 132.88, 132.74, 130.78, 130.66, 128.59, 128.49, 128.44, 128.25, 127.28, 125.50, 58.58, 29.99, 16.90. 31P-NMR (500 MHz, CDCl3): -19.04 (s, 1P). GC/MS: 363 (2%, M+), 348 (2%, [M-15]+), 320 (100%, [M-43]+), 288 (10%), 214 (12%), 183 (39%), 121 (20%), 108 (42%). Under argon dichlorotris(triphenylphosphine)ruthenium(ll) (0.53 g, 0.55 mmol) is added to a solution of 2-(diphenylphosphino)-N-(2-(methylthio)benzylidene)ethanamine (0.20 g, 0.55 mmol) in toluene (15 ml). After stirring for 20 h at 110 C the reaction mixture is cooled to room temperature and evaporated under vacuo to a volume of 5 ml. To this red suspension hexane (20 ml) is added. After stirring for 15 min the suspension is filtered and 15 washed with hexane (4 ml). The red filter cake is dried under vacuo for 19 h and then suspended in diethyl ether (6 ml). The suspension is filtered, washed with diethyl ether (4 x 4 ml) and the filter cake is dried under vacuo. Complex 8 is obtained as a light-red solid (0.29 g, 67%). Analytical data: 1H-NMR (400 MHz, CDCl3): 8.78 (d, 7=8.84, 1H), 8.33 (m, 1H), 7.70 (m, 3H), 7.54-7.06 (m, 20 25H), 4.59 (m, 1H), 4.53 (m, 1H), 2.55 (m, 2H), 1.83 (d, 7=2.53, 3H). 31P-NMR (500 MHz, CDCl3): 40.62 (d, 7=32.27, IP), 36.72 (d, 7=32.37, IP). MS (ESI): 797.18 (62%, M+), 762.12 (100%, [M-Cl]+).

With the rapid development of chemical substances, we look forward to future research findings about Dichlorotris(triphenylphosphino)ruthenium (II)

Reference£º
Patent; GIVAUDAN SA; GEISSER, Roger Wilhelm; OETIKER, Juerg Daniel; SCHROeDER, Fridtjof; WO2015/110515; (2015); 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.246047-72-3,(1,3-Bis(2,4,6-trimethylphenyl)-2-imidazolidinylidene)dichloro(phenylmethylene)(tricyclohexylphosphine)ruthenium,as a common compound, the synthetic route is as follows.

After a 50 mL two-necked flask was purged with argon, the ligand 3bv (10 mmol), CuCl (30 mmol, 3 eq) and 30 mL of dry DCM were sequentially added and the mixture was purged three times with argon to protect the closed system with argon balloon. Ruthenium complex 1b (12 mmol) was added under argon atmosphere, and the reaction was carried out at room temperature for 0.5 hour. After the reaction was completed, silica gel was added to the filtrate to prepare a sand product. The crude product was obtained by silica gel column chromatography, and then washed with methanol or pentane-DCM to obtain a green solid product 4bv. Yield: 90%., 246047-72-3

The synthetic route of 246047-72-3 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Zannan Science And Technology (Shanghai) Co., Ltd.; Zhan Zhengyun; (102 pag.)CN104262403; (2017); B;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Dichlorotris(triphenylphosphino)ruthenium (II), cas is 15529-49-4, it is a common heterocyclic compound, the ruthenium-catalysts compound, its synthesis route is as follows.,15529-49-4

A 50 ml three-necked flask equipped with a stirring reflux device was charged with 1 mmol of 2-diethylphosphine aniline,1.3 mmol of o-methoxybenzyl alcohol, 1 mmol2-dicyclohexylphosphine oxide, 1 mmol RuCl2 (PPh3) 3, 1.1 mmol potassium hydroxide, 20 ml benzene and heating at a temperature of 100 C for 18 h under a nitrogen atmosphere,After cooling and filtering, the resulting solid was recrystallized from a mixed solvent of CH 2 Cl 2 and petroleum ether to give product 15 in a yield of 80%.

As the rapid development of chemical substances, we look forward to future research findings about 15529-49-4

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

Dichlorotris(triphenylphosphino)ruthenium (II), cas is 15529-49-4, it is a common heterocyclic compound, the ruthenium-catalysts compound, its synthesis route is as follows.,15529-49-4

To Hpytol (0.12 g,0.5 mmol) in methanol (10 mL), [RuCl2(PPh3)3] (0.23 g, 0.25 mmol) in methanol (5 mL) was added. The reaction was carried out in presence of Et3N (0.05 mL, 0.5 mmol). The mixture was heated under reflux for 1.5 h, during which a deep red precipitate was obtained. It was filtered off, washed with methanol and ether, then dried in vacuo, Yield, 88%; mp 300 C. LM inCH2Cl2 3 U1 cm2 mol1. Elemental Anal. Calcd. ForC66H60N4O4RuP2: C, 69.7; H, 5.3; N, 4.9%. Found: C, 69.5; H, 5.0; N,4.8%. IR (KBr, cm1): n (OeH) 3407(m,b), n (C]N) 1625, n (CeO)1285(s), n(PPh3) 1091(s), n(RueO) 522(m), n (RueN) 460 (m). 1HNMR (DMSO-d6,d/ppm): 8.57 (HC]N), 1H, s); 8.1(H6), 1H, s);7.33e7.44 (Ph-H, 4H, m); 5.07 (CH2, 2H, s); 4.37 (OHCH2OH, 1H, s);2.3 (CH3, 3H, s).

As the rapid development of chemical substances, we look forward to future research findings about 15529-49-4

Reference£º
Article; Elsayed, Shadia A.; Noufal, Aya M.; El-Hendawy, Ahmed M.; Journal of Molecular Structure; vol. 1144; (2017); p. 120 – 128;,
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.246047-72-3,(1,3-Bis(2,4,6-trimethylphenyl)-2-imidazolidinylidene)dichloro(phenylmethylene)(tricyclohexylphosphine)ruthenium,as a common compound, the synthetic route is as follows.

Grubbs second generation catalyst (100 mg, 0.118 mmol) andacrylonitrile (25 mg, 0.472 mmol) were stirred in toluene (5 mL) for15 h at room temperature. After removal of volatiles by evacuation,the brown powder was washed with pentane (3 ¡Á 5 mL) and driedunder vacuum, affording 7-CN as a brown solid in a 80% yield, 246047-72-3

246047-72-3 (1,3-Bis(2,4,6-trimethylphenyl)-2-imidazolidinylidene)dichloro(phenylmethylene)(tricyclohexylphosphine)ruthenium 11147261, aruthenium-catalysts compound, is more and more widely used in various fields.

Reference£º
Article; Vancompernolle, Tom; Vignon, Paul; Trivelli, Xavier; Mortreux, Andre; Gauvin, Regis M.; Catalysis Communications; vol. 77; (2016); p. 75 – 78;,
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.15529-49-4,Dichlorotris(triphenylphosphino)ruthenium (II),as a common compound, the synthetic route is as follows.

Example 9: Dichloro[2-(diphenylphosphino)-N-(2-(methylthio)benzyl)ethanamine]ruthenium(ll) (9) Under argon NaBH4 (0.13 g, 3.47 mmol) is added to a solution of 2-(diphenylphosphino)-N- (2-(methylthio)benzylidene)ethanamine (0.42 g, 1.16 mmol) in ethanol (7 ml). After stirring for 20 h at 80 C the reaction mixture is cooled to room temperature and DCM (10 ml) is added, followed by saturated aqueous NH4Cl-solution. The phases were separated and 5 the organic phase is washed twice with water and once with brine. The organic phase is dried over MgSO4, filtered and concentrated under vacuo. Ligand 2-(diphenylphosphino)- N-(2-(methylthio)benzyl)ethanamine is obtained as a yellow liquid (0.36 g, 86%). Analytical data: 1H-NMR (400 MHz, CDCl3): 7.76 (m, 1H), 7.44 (m, 4H), 7.34 (m, 6H), 7.24 (m, 2H), 7.12 (m, 1H), 3.86 (s, 2H), 2.81 (m, 2H), 2.49 (s, 3H), 2.34 (m, 2H), 1.75 (bs, 1H). 13C-NMR (400 MHz, CDCl3): 138.89, 138.25, 137.70, 133.13, 129.29, 128.95, 128.82, 128.05, 126.09, 125.31, 51.88, 46.43, 29.48, 16.17. 31P-NMR (500 MHz, CDCl3): -20.60 (s, IP). GC/MS: 350 (16%, [M-15]+), 318 (40%), 200 (26%), 183 (32%), 166 (11%), 152 (19%), 137 (100%), 121 (33%), 15 108 (36%), 91 (25%), 77 (13%), 45 (28%). Under argon dichlorotris(triphenylphosphine)ruthenium(ll) (0.94 g, 0.99 mmol) is added to a solution of 2-(diphenylphosphino)-N-(2-(methylthio)benzyl)ethanamine (0.36 g, 0.99 mmol) in toluene (20 ml). After stirring for 19 h at 110 C the reaction mixture is cooled to room temperature and evaporated under vacuo to a volume of 5 ml. To this suspension 20 hexane (20 ml) is added. After stirring for 15 min the suspension is filtered and washed with hexane (4 ml) and diethyl ether (2 x 4 ml). The light-brown filter cake is dried under vacuo for 19 h and then suspended in diethyl ether (5 ml). After stirring for 15 min the suspension is filtered, washed with diethyl ether (3 x 1 ml) and the filter cake is dried under vacuo. Complex 9 is obtained as a light-brown solid (0.76 g, 96%). Analytical data: 1H-NMR (400 MHz, CDCl3): 7.80 (m, 6H), 7.69 (m, 1H), 7.47 (m, 3H), 7.31-7.01 (m, 17H), 6.88 (dt, 7=2.02, 7.58, 1H), 7.18 (d, 7=7.33, 1H), 5.48 (bs, 1H), 5.23 (d, 7=12.63, 1H), 4.11 (m, 1H), 3.89 (m, 1H), 3.00 (m, 1H), 2.07 (m, 1H), 1.12 (m, 1H), 1.08 (s, 3H). 31P-NMR (500 M Hz, CDCl3): 49.83 (d, 7=27.74, 1P), 37.96 (d, 7=27.74, 1P). Anal, calcd. for C40H39Cl2NP2R11S: C, 60.07 %; H, 4.92 %; N, 1.75 %. Found : C, 60.36 %; H, 4.79 %; N, 1.47 %., 15529-49-4

The synthetic route of 15529-49-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; GIVAUDAN SA; GEISSER, Roger Wilhelm; OETIKER, Juerg Daniel; SCHROeDER, Fridtjof; WO2015/110515; (2015); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Dichlorotris(triphenylphosphino)ruthenium (II), cas is 15529-49-4, it is a common heterocyclic compound, the ruthenium-catalysts compound, its synthesis route is as follows.,15529-49-4

A mixture of HL1 (80mg, 0.20mmol), triethylamine (20mg, 0.20mmol) and 1[Ru(PPh3)3Cl2] (192mg, 0.20mmol) were stirred in tetrahydrofuran (20mL) for 6h at room temperature, during which the color of solution changed from brown to dark red. After removal of solvents in vacuo, dichloromethane (20mL) was added and the solution was filtered. The filtrate was concentrated and the residue was washed with diethyl ether (5mL¡Á2) and hexane (5mL¡Á2) to give the desired product. Recrystallization from dichloromethane/hexane (1:3) afforded dark red block crystals of [Ru(L1)(PPh3)2Cl] (1) suitable for X-ray diffraction in three days. Yield: 140mg, 66% (based on ruthenium). IR (KBr disc, cm-1): nuC=N 1568 (m), nuC-O 1304 (s), nuC-S 744 (w), nuPPh3 1433(m), 1091(s) and 694 (w), nuC-Br 564 and 529 (s); 31P NMR (CDCl3, 162MHz): delta 17.0 (s, PPh3) ppm. 1H NMR (CDCl3, 400MHz): delta 9.82 (s, 1H, CH=N), 7.91-7.52 (m, 30H, PPh3), 7.21-7.10 (m, 2H, Ar-H), 6.35-6.20 (m, 4H, Ar-H), 2.17 (s, 3H, SCH3) ppm. MS (FAB): m/z 1061 [M+], 1026 [M+-Cl], 799 [M+-PPh3], 537 [M+-2PPh3], 513 [Ru(L1)]+. Anal. Calc. for C50H40NOP2ClBr2SRu: C, 56.59; H, 3.80; N, 1.32%. Found: C, 56.54; H, 3.83; N, 1.36%.

As the rapid development of chemical substances, we look forward to future research findings about 15529-49-4

Reference£º
Article; Ji, Jiao; Chen, Xin; Lin, Hui; Jia, Ai-Quan; Zhang, Qian-Feng; Inorganica Chimica Acta; vol. 494; (2019); p. 105 – 111;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI