Downstream synthetic route of Dichlorotris(triphenylphosphino)ruthenium (II), As a common heterocyclic compound, it belongs to ruthenium-catalysts compound, name is Dichlorotris(triphenylphosphino)ruthenium (II), and cas is 15529-49-4, its synthesis route is as follows.
A Schlenk flask was loaded with [Ru(PPh3)3(Cl)2] (2.0270 g,2.114 mmol) and bis(3-aminopropyl)phenylphosphine (1) (0.4816 g,2.147 mmol), to which was added 17 ml of anhydrous toluene to generate a yellow suspension. The mixture was stirred in an oil bath at 110 C, for two hours. The yellow suspension was then stirred for 16 h at room temperature, after which time the solid was isolated via canula filtration and washed with 100 ml of anhydrous diethyl ether 3 times. The solid was dried under vacuum for 72 h. Isolated mass 1.20 g, 86% yield. NMR data – 1H NMR (CDCl3, delta): 7.71 (m with appearance of t,6 H) 7.43 (m with appearnce of t, 2 H), 7.14-6.94 (m, 10 H), 6.88 (mwith appearance of t, 2 H) 4.25, (br, 2H, NH), 3.39 (br, 2H, NH and CH),3.08 (br, 1H, CH), 2.23-1.81 (m, 10H, 9CH and NH), 0.68 (br, 1H, CH). 13C{1H} NMR (CDCl3, delta): 138.7 (d, i-C of PPh), 137.0 (d, i-C of PPh3),134.0 (d, o-C of PPh3), 131.2 (d, o-C of PPh), 128.4 (s, p-C of PPh3),128.2 (s, p-C of PPh), 127.7 (d, m-C of PPh), 127.5 (d, m-C of PPh3),42.3, 40.5, 33.3 (d, 1JPC=26.9 Hz), 27.9 (d, 1JPC=27.8 Hz), 26.1,25.4. 31P{1H} NMR (CDCl3, delta): 48.8 (d, 2JPP=34 Hz), 32.65 (d,2JPP=34 Hz). Elemental analysis calculated (%) for C30H36Cl2N2P2Ru:C 53.93, H 5.51, N 4.25; found: C 53.72, H 5.51, N 4.52 Product is soluble in dichloromethane and chloroform, but insoluble in methanol,ethanol, isopropanol and acetonitrile. The product is air sensitive in solution, turning green on exposure to air. A sample of the solid exposed to air for 2 h and returned to the glove box was analysed by NMR; no new unassigned signals were observed in either the 1H or 31P NMR spectra. Single crystals of [Ru(1)PPh3(Cl)2] were grown by layering hexane onto a DCM solution of the complex to enable slow diffusion of the solvents
15529-49-4, In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles.,15529-49-4 ,Dichlorotris(triphenylphosphino)ruthenium (II), other downstream synthetic routes, hurry up and to see
Reference£º
Article; Braden, Drew J.; Cariou, Renan; Shabaker, John W.; Taylor, Russell A.; Applied Catalysis A: General; vol. 570; (2019); p. 367 – 375;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI