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.
1-(isopropylsulfanyl)-2-vinylbenzene (25.0 mg, 0.14 mmol), cuprous chloride (16.7 mg, 0.17 mmol) and (1,3-Bis(2,4,6-trimethylphenyl)-2-imidazolidinylidene)dichloro(phenylmethylene)(tricyclohexylphosphine)ruthenium (119 mg, 0.14 mmol) were dissolved in 6 mL dichloromethane in a 10 mL round-bottomed flask under dry nitrogen topped with a reflux condenser. The reaction mixture was refluxed for 4.5 h. The resulting mixture was evaporated to dryness. The crude product was purified by chromatography on silica gel using 7:3 n-hexane and acetone as eluent to give a teal solid (48.0 mg, 55%). Two additional byproducts were separated by chromatography, but only one was fully characterized by NMR analysis: the trans-catalyst isomer green solid (8.1 mg, 9%) and additional green solid (14.2 mg). Both spontaneously converted with time to product 1A according to NMR analysis. Crystals suitable for X-ray analysis were obtained by laying hexanes over a solution of 1A in dichloromethane for few days at -18 C. [0056] 1H NMR (500 MHz, CD2Cl2): delta 0.76 (d, J=6.5 Hz, 3H), 1.41 (d, J=7.4 Hz, 3H), 1.56 (s, 3H), 2.16 (s, 3H), 2.37 (s, 3H), 2.44 (s, 3H), 2.57 (s, 3H), 2.64 (s, 3H), 3.58 (m, 1H), 3.80 (m, 1H), 3.88 (m, 1H), 4.00 (m, 1H), 4.11 (m, 1H), 5.96 (bs, 1H), 6.79 (d, J=7.5 Hz, 1H), 6.88 (bs, 1H), 7.04 (bs, 1H), 7.12 (bs, 1H), 7.17 (t, J=6.4 Hz, 1H), 7.46 (m, 2H), 17.14 (s, 1H) ppm. 13C NMR (125 MHz, CDCl3): delta 17.7, 18.7, 19.7, 20.3, 20.9, 21.0, 21.3, 24.2, 39.0, 51.4, 51.6, 123.7, 128.6, 129.4, 129.6, 129.7, 129.8, 130.7, 131.7, 135.0, 135.4, 135.6, 137.3, 137.7, 138.5, 140.3, 140.4, 156.6, 213.6, 285.6 ppm. APCI-MS m/z (M-Cl)+: 607.1 (Calc. 607.15).
246047-72-3, As the paragraph descriping shows that 246047-72-3 is playing an increasingly important role.
Reference£º
Patent; LEMCOFF, N. Gabriel; BEN-ASULY, Amos; US2014/155511; (2014); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI