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.
cis-cis- 1,3,5-triaminocyclohexane (30.0 nig, 0.232 mmol) was added to an ampoule charged with dichlorotris(triphenylphosphane)ruthenium(II) (196 mg, 0.204 mmol) dissolved in dichloromethane (20 mL), causing an instant colour change from black to orange. The solution was stirred at 50C for 4 days in the sealed vessel, during whichtime the solution changed colour to yellow and a white precipitate formed. The precipitate was removed by filtration and the filtrate reduced in volume to approx. 1 mL in vacuo. The product was precipitated by addition of pentane (20 mL) as an orange powder, and washed twice with pentane (20 mL). Yield: 115 mg (86.8 %, 0.177 mmol of RuCl2(K3-c -tach)(PPh3).CH2Cl2). NMR Spectroscopy Cs minor plane H NMR (CD2C12, 399.8 MHz, 293K) delta 7.85 (app t, HH = 7.5 Hz, VHP = 5.8 Hz, VHH = 1.5 Hz, 6H, P/Vz3, Ar2), 7.36 (m, 9H, Rho/>Lambda3, Ar3 + Ar4), 4.77 (s, 2H, NH2, N1), 3.90 (bs, 1Eta, CH, Cy1), 2.92 (s, 2Eta, CH, Cy2), 2.65 (d, VHH = 10.6 Hz, 2H, N N2), 1.92 (s, 4H, CH2, Cy3), 1.85 (d, HH = 10.6 Hz, 2H, NH2, N2), 1.62 (d, VHH = 15.3 Hz, 1H, CH2, Cy4), 1.00 (d, VHH = 15.3 Hz, 1H, CH2, Cy4); 31Rho{} NMR (CD2C12, 161.8 MHz, 293 ) delta 66.0 (s, IP, PPh3); “Ci’H} NMR (CD2C12, 100.5 MHz, 293K) delta 136.2 (d, ‘Jpc = 36.0 Hz, VPh3, Ar1), 134.2 (d, VPC = 10.1 Hz, VPh3, Ar2), 129.5 (d, VPC = 1.85 Hz, ?P 3, Ar4), 128.8 (d, VPC = 8.7 Hz, ?Ph3, Ar3), 44.0 (s, CH, Cy1), 43.8 (s, CH, Cy2), 35.0 (s, CH2, Cy3), 33.6 (s, CH2, Cy4).Mass Spectrometry ESI-MS: m/z 569.1186 ([RuCl(NCMe)( 3-c i-tach)(PPh3)l+. Calc 569.1173, 100 %), 528.0919 ([RuCl(K3-c-tach)(PPh3)]+; 528.0907, 25), 246.5607 ([RU(K3-CW- tach)(PPh3)]2+, 246.5608, 10). Infra-Red Spectroscopy ATR-IR: (cm 1) 3462, 3283, 3240, 3050, 2888, 1649, 1588, 1480, 1432 (P-Ph), 1367, 1346, 1270, 1211, 1183, 1156, 1089, 1027, 968, 905. Elemental Analysis CH2C12 c / % H / % N / % Found 46.25 4.92 6.43 0 51.15 5.37 7.46 1 46.31 4.97 6.48 Table 0.1: CHN Elemental analysis for RuCl2(K3-cw-tach)(PPh3)
As the paragraph descriping shows that 15529-49-4 is playing an increasingly important role.
Reference£º
Patent; UNIVERSITY OF YORK; GAMBLE, Aimee, Joanna; LYNAM, Jason, Martin; WALTON, Paul, Howard; WO2013/38134; (2013); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI