As a common heterocyclic compound, it belongs to quinuclidine compound,Quinuclidine-4-carboxylic acid hydrochloride,40117-63-3,Molecular formula: C8H14ClNO312,mainly used in chemical industry, its synthesis route is as follows.,15529-49-4
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
With the synthetic route has been constantly updated, we look forward to future research findings about Dichlorotris(triphenylphosphino)ruthenium (II),belong ruthenium-catalysts compound
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