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.
A Schlenk flask was loaded with [Ru(PPh3)3(Cl)2] (1.2156 g,1.268 mmol) and 2,6-bis(2-benzimidazolyl)pyridine (4) (0.4088 g,1.313 mmol), to which was added 25 ml of anhydrous toluene. The mixture was stirred in an oil bath at 110 C, for two hours, during which time a red-brown precipitate had formed. The 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 1.07 g, 84% yield. NMR data – 1H NMR (d4-methanol, delta):8.53 (m, 2 H), 7.60 (t, J=8.0 Hz, 1 H), 7.40 (m, 8 H), 7.13 (m, 18H,PPh3), 6.88 (t, J=7.7 Hz, 12H, PPh3), NH signals not observed due to rapid H/D exchange with CD3OD. 13C{1H} NMR (d4-methanol, delta):152.7, 152.1, 144.1 and 135.7 (quaternary C), 134.4 (t, o-C of PPh3),133.3 (aromatic CeH), 132.4 (t, i-C of PPh3),130.4 (s, p-C of PPh3),128.8 (t, m-C of PPh3), 126.8, 124.5, 122.9, 122.1 and 113.6 (aromaticCeH). 31P{1H} NMR (d4-methanol, delta): 22.1 (s). Elemental analysis calculated (%) for C55H43Cl2N5P2Ru: C 65.54, H 4.30, N 6.95; found: C65.40, H 4.42, N 7.03. Product is soluble in methanol, poorly soluble in ethanol, but insoluble in acetone, acetonitrile and dichloromethane. A d4-MeOH NMR sample exposed to air was observed to form crystal safter 3 h. However, no decomposition signals were observed in the NMR spectrum. A sample of the solid exposed to air for 2 h and returned to the glove box was analysed by NMR; new unassigned signals appeared in both the 1H and 31P NMR spectra
15529-49-4, The synthetic route of 15529-49-4 has been constantly updated, and we look forward to future research findings.
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