With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.203714-71-0,Dichloro(2-isopropoxyphenylmethylene)(tricyclohexylphosphine)ruthenium (II),as a common compound, the synthetic route is as follows.
In a glove box, NHC ligand precursor 23 (63 mg, .13, mmol), ruthenium precursor 11 (78 mg, .13 mmol) and KOMJu(Fe) (29 mg, .13 mmol) were combined in toluene. The flask was sealed, removed from the glove box and stirred at 60 0C for 18 hours. The reaction was concentrated and purified by flash column chromatography (5% –> 20% Et2O/Pent). There were 3 bands that could be isolated from this column, first 2 brown bands and then one green band. The second brown band was the desired product; however, it was not completely pure after one column. Recolumning in 10% Et2O/Pentane gave a brown oil product completely pure by 1H NMR (9 mg, 9%) and another fraction still slightly impure (18 mg, 18%). The products were lyophilized from benzene to give solids. 1H NMR (300 MHz, CDCl3) delta 16.78 (s, IH), 8.13 (br, 2H), 7.74-7.62 (m, 4H), 7.07-7.04 (m, IH), 6.97 (dd, J = 3, 1.5 Hz, IH), 6.66 (t, J = 7.5 Hz, 3H), 6.34 (d, J = 8.4 Hz, IH), 4.49 (sept, J = 6 Hz, IH), 1..44 (d, J = 6 Hz, 6H), 1.44 (br, 18H), 1.18 (br, 18H); 13C (75 MHz, CDCl3) delta; HRMS (EI+) calc for C4IH56Cl2N2ORu, 764.2814. Found 764.2842.
As the paragraph descriping shows that 203714-71-0 is playing an increasingly important role.
Reference£º
Patent; MATERIA, INC.; CALIFORNIA INSTITUTE OF TECHNOLOGY; WO2007/75427; (2007); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI