15529-49-4, Dichlorotris(triphenylphosphino)ruthenium (II) is a ruthenium-catalysts compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
In a 3 L, 3-neck round bottom flask were added C959 (100.0 g, 104.2 mmol), 1,1- diphenyl-2-propyn-1-ol (24.9 g, 119.8 mmol), and triphenylphosphine (27.3 g, 104.2 mmol) under air. The flask was equipped with a thermocouple and rubber suba-seal septum and then it was placed under Ar using Schlenk technique. The reagents and products of this reaction are highly air sensitive in solution. A 1 L addition funnel was attached to the flask under a flow of Ar. To the addition funnel were added (2-Me)THF (1 L) and 4 M HC1 (25.6 mL, 104.2 mmol) in dioxane using Schlenk technique. The solution was added over 10 minutes at room temperature with stirring. Another 0.75 L (2-Me)THF were added directly to the flask. The addition funnel was replaced with a glass stopper under a flow of Ar and the flask was lowered into a pre-heated oil bath at 65 C. The reaction was monitored by 31P NMR. When conversion was deemed to be complete, the reaction flask was removed from the oil bath and hot filtered via cannula transfer through a celite pad (in an evacuated Schlenk filter) into a Schlenk flask. Approximately 85% (2- Me)THF was removed at room temperature (water bath) under vacuum. The resulting slurry was cooled to 0 C then filtered on a coarse glass frit under air. The solid was washed quickly with 3×50 mL portions of 0 C (2-Me)THF followed by hexanes (200 mL) (r.t.) and 2-propanol (100 mL). The solid from the frit was re-slurred with hexanes (200 mL) and filtered again. The solid was air-dried until no condensation was seen on the outside of the glass frit, then transferred to a 200 mL round bottom flask and dried under high vacuum overnight. The final ?H NMR andNIVIR in CDC13 indicate that the complex is a 1:1 adduct of (PPh3)2Ru(Phlnd)C12, and (2- Me)THF, C973, for a final molecular weight of 973 g/mol. Yield = 74.1 g (73%). 1H NMR (400 MFIz in CDC13 at r.t.): = 7.2-7.6 (overlapping CDC13 andaromatics), 7.07 (d, md, 1H), 6.62 (t, md, 1H), 6.43 (s, md, 1H), 3.92 (m, (2-Me)THF, 2H), 3.70(m, (2-Me)THF, 1H), 1.88-1.98 (overlapping m, (2-Me)THF, 3H), 1.41 (m, (2-Me)THF, 1H), 1.23(d, (2-Me)THF, 3H).
As the paragraph descriping shows that 15529-49-4 is playing an increasingly important role.
Reference£º
Patent; MATERIA, INC.; CALIFORNIA INSTITUTE OF TECHNOLOGY; JOHNS, Adam, M.; HERRON, Jessica, R.; PEDERSON, Richard, L.; FIAMENGO, Bryan, A.; BEERMAN, Jennifer, A.; LIN, Tzu-Pin; CHU, Crystal, K.; GRUBBS, Robert, H.; (104 pag.)WO2018/75479; (2018); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI