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.
Example 9: Dichloro[2-(diphenylphosphino)-N-(2-(methylthio)benzyl)ethanamine]ruthenium(ll) (9) Under argon NaBH4 (0.13 g, 3.47 mmol) is added to a solution of 2-(diphenylphosphino)-N- (2-(methylthio)benzylidene)ethanamine (0.42 g, 1.16 mmol) in ethanol (7 ml). After stirring for 20 h at 80 C the reaction mixture is cooled to room temperature and DCM (10 ml) is added, followed by saturated aqueous NH4Cl-solution. The phases were separated and 5 the organic phase is washed twice with water and once with brine. The organic phase is dried over MgSO4, filtered and concentrated under vacuo. Ligand 2-(diphenylphosphino)- N-(2-(methylthio)benzyl)ethanamine is obtained as a yellow liquid (0.36 g, 86%). Analytical data: 1H-NMR (400 MHz, CDCl3): 7.76 (m, 1H), 7.44 (m, 4H), 7.34 (m, 6H), 7.24 (m, 2H), 7.12 (m, 1H), 3.86 (s, 2H), 2.81 (m, 2H), 2.49 (s, 3H), 2.34 (m, 2H), 1.75 (bs, 1H). 13C-NMR (400 MHz, CDCl3): 138.89, 138.25, 137.70, 133.13, 129.29, 128.95, 128.82, 128.05, 126.09, 125.31, 51.88, 46.43, 29.48, 16.17. 31P-NMR (500 MHz, CDCl3): -20.60 (s, IP). GC/MS: 350 (16%, [M-15]+), 318 (40%), 200 (26%), 183 (32%), 166 (11%), 152 (19%), 137 (100%), 121 (33%), 15 108 (36%), 91 (25%), 77 (13%), 45 (28%). Under argon dichlorotris(triphenylphosphine)ruthenium(ll) (0.94 g, 0.99 mmol) is added to a solution of 2-(diphenylphosphino)-N-(2-(methylthio)benzyl)ethanamine (0.36 g, 0.99 mmol) in toluene (20 ml). After stirring for 19 h at 110 C the reaction mixture is cooled to room temperature and evaporated under vacuo to a volume of 5 ml. To this suspension 20 hexane (20 ml) is added. After stirring for 15 min the suspension is filtered and washed with hexane (4 ml) and diethyl ether (2 x 4 ml). The light-brown filter cake is dried under vacuo for 19 h and then suspended in diethyl ether (5 ml). After stirring for 15 min the suspension is filtered, washed with diethyl ether (3 x 1 ml) and the filter cake is dried under vacuo. Complex 9 is obtained as a light-brown solid (0.76 g, 96%). Analytical data: 1H-NMR (400 MHz, CDCl3): 7.80 (m, 6H), 7.69 (m, 1H), 7.47 (m, 3H), 7.31-7.01 (m, 17H), 6.88 (dt, 7=2.02, 7.58, 1H), 7.18 (d, 7=7.33, 1H), 5.48 (bs, 1H), 5.23 (d, 7=12.63, 1H), 4.11 (m, 1H), 3.89 (m, 1H), 3.00 (m, 1H), 2.07 (m, 1H), 1.12 (m, 1H), 1.08 (s, 3H). 31P-NMR (500 M Hz, CDCl3): 49.83 (d, 7=27.74, 1P), 37.96 (d, 7=27.74, 1P). Anal, calcd. for C40H39Cl2NP2R11S: C, 60.07 %; H, 4.92 %; N, 1.75 %. Found : C, 60.36 %; H, 4.79 %; N, 1.47 %., 15529-49-4
The synthetic route of 15529-49-4 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; GIVAUDAN SA; GEISSER, Roger Wilhelm; OETIKER, Juerg Daniel; SCHROeDER, Fridtjof; WO2015/110515; (2015); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI