With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.301224-40-8,(1,3-Dimesitylimidazolidin-2-ylidene)(2-isopropoxybenzylidene)ruthenium(VI) chloride,as a common compound, the synthetic route is as follows.
Hoveyda-Grubbs second generation catalyst H2 (104 mg, 0.16 mmol) and potassium 2,6-dimethylbenzenethiolate (34 mg, 0.19 mmol) 2b were transferred to a 25 mL Schlenk flask, followed by addition of 4 mL of toluene and 1 mL THF under argon. Then the mixture was stirred vigorously at 20 C. for 30 min. During this time the color of the mixture turned from light green to a slightly darker green. The reaction mixture was filtered, and the volume of the filtrate reduced to about 3 mL. Hexane (15 mL) was added to the filtrate to precipitate the product 4b as red/orange-brown micro-crystals (86.3 mg, 71%). (0121) Crystals for X-ray diffraction analysis (see FIG. 12 and Table 4) were prepared by dissolving a sample in a minimal amount of toluene, upon which a layer of hexane was added. Red-brown crystals were formed over a period of 3 days at room temperature. (0122) 1H NMR (400.13 MHz, CDCl3): delta=14.90 (s, 1H), 7.22 (m, 1H), 7.10 (s, 2H), 7.06 (s, 2H), 6.80-6.73 (m, 2H), 6.66 (t, J=7.2 Hz, 1H), 6.16 (d, J=8.0 Hz, 1H), 4.15 (m, 4H), 3.83 (sep, J=6.16 Hz, 1H), 2.62 (s, 6H), 2.54 (s, 6H), 2.42 (s, 6H), 2.32 (br s, 3H), 1.8 (d, J=5.6 Hz, 3H), 0.89 (d, J=6.4 Hz, 3H), 0.80 (br s, 3H). 13C NMR (100.6 MHz, CDCl3): delta=271.29, 211.87, 151.57, 145.12, 142.30 (br), 141.67, 139.25, 138.90, 138.75, 137.40 (br), 129.74, 129.43, 127.32, 126.61, 124.43, 123.12, 122.34, 114.19, 74.99, 52.15, 21.55, 21.45, 21.43, 20.07 (br). (0123) A corresponding ORTEP-style diagram of 4b is shown in FIG. 12. Selected geometrical parameters: Ru1-C9=1.846 , Ru1-S1=2.285 , Ru1-Cl1=2.364 , Ru1-O1=2.298 , Ru1-S1-C1=113.67, Cl1-Ru1-S1=150.75.
The synthetic route of 301224-40-8 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; Bergen Teknologioverforing AS; Jensen, Vidar R.; Occhipinti, Giovanni; Hansen, Frederick Rosberg; US8716488; (2014); B2;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI