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CAS No. : | 15243-33-1 | MDL No. : | MFCD00011209 |
Formula : | C12O12Ru3 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 639.33 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P304+P340 | UN#: | |
Hazard Statements: | H332 | Packing Group: | |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
81.9% | In tetrahydrofuran;Reflux; Inert atmosphere; | Add 2-(6-bromopyridinyl)-isopropanol to a 100 mL flask(0.20 g, 0.94 mmol) and Ru3(CO)12 (0.30 g, 0.47 mmol),Then, 30 mL of anhydrous tetrahydrofuran was added, and the mixture was heated under reflux for 24 hours under nitrogen. After the reaction was completed, it was cooled to room temperature, and the solvent was removed under reduced pressure.Neutral alumina was passed through the column to finally obtain a yellow solid of 0.30 g.The yield was 81.9%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
12% | In dichloromethane; at 40℃; for 8h;Inert atmosphere; Schlenk technique; | A CH2Cl2 solution (20mL) of [Ru3(CO)12] (100mg, 0.16mmol) and tsacH (63mg, 0.32mmol) was heated to reflux for 8h during which time the color of the solution changed from yellow to deep red. The reaction mixture was then allowed to cool at room temperature, and the solvent was removed under reduced pressure. The residue was separated by TLC on silica gel using a binary eluent composed of n-hexane/CH2Cl2 (v/v, 1:1), yielding a single yellow band corresponding to [Ru2(CO)6(mu-N,S-tsac)2] (1). The product was recrystallized from n-hexane/CH2Cl2 at 4C and furnished orange crystals of analytically pure 1 in 12% yield (14mg). Data for 1: Anal. Calc. for C20H8N2O10Ru2S4: C, 31.33; H, 1.05; N, 3.65. Found: C, 31.64; H, 1.12; N, 3.69%. IR (nuCO, CH2Cl2): 2102s, 2075vs, 2032sh, 2027s, 1961w cm-1. 1H NMR (CDCl3): delta 8.01 (d, J 7.2Hz, 2H), 7.88 (d, J 7.2Hz, 2H), 7.78 (t, J 7.2Hz, 2H), 7.73 (t, J 7.2Hz, 2H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
4%; 17%; 7%; 11% | In tetrahydrofuran; at 66℃; for 4h;Inert atmosphere; Schlenk technique; | To a thf solution (20mL) of [Ru3(CO)12] (100mg, 0.16mmol) was added tsacH (63mg, 0.32mmol). The reaction mixture was heated to reflux for 4h, after which time the reaction mixture was then allowed to cool at room temperature. The solvent was removed under reduced pressure and the residue chromatographed by TLC on silica gel. Elution with n-hexane/CH2Cl2 (v/v, 1:1) developed four bands. The first band was unreacted [Ru3(CO)12] (14mg). The second band afforded [H2Ru3(CO)7(mu-N,S-tsac)(mu-C,N-C6H4CNSO2)(mu3-S)] (2) as orange crystals (24mg, 17%) after recrystallization from n-hexane/CH2Cl2 at 4C. The third band afforded two types of crystals (yellow and orange) after recrystallization from n-hexane/CH2Cl2 at 4C which were physically separated by hand. The orange crystals were characterized as [Ru2(CO)6(mu-N,S-tsac)2] (1) (7mg, 4%), while the yellow crystals were characterized as [Ru4(CO)12(mu-N,S-tsac)2(mu4-S)] (3) (10mg, 7%). The fourth band afforded [H2Ru5(CO)13(mu-N,S-tsac)(mu-C,N-C6H4CNSO2)(mu3-S)(mu4-S)] (4) (14mg, 11%) as orange crystals after recrystallization from n-hexane/CH2Cl2 at 4C. Data for 2: Anal. Calc. for C21H10N2O11Ru3S4: C, 28.10; H, 1.12; N, 3.12. Found: C, 28.32; H, 1.15, N, 3.14%. IR (nuCO, CH2Cl2): 2124vs, 2067vs, 2060sh, 2012s cm-1. 1H NMR (CDCl3): delta 8.29 (d, J 8.0Hz, 1H), 8.02 (m, 1H), 7.91 (t, J 7.2Hz, 1H), 7.85 (m, 1H), 7.82 (m, 1H), 7.78 (d, J 7.2Hz, 1H), 7.73 (m, 2H),-14.31 (d, J 0.8Hz, 1H),-16.14 (d, J 0.8Hz, 1H). Data for 3: Anal. Calc. for C26H8N2O16Ru4S5: C, 26.72; H, 0.69; N, 2.40. Found: C, 27.08; H, 0.74; N, 2.48%. IR (nuCO, CH2Cl2): 2124w, 2102s, 2087vs, 2066vs, 2021vs cm-1. 1H NMR (CD2Cl2): delta 8.06 (m, 1H), 7.99 (d, J 7.2Hz, 1H), 7.90-7.76 (m, 6H). Data for 4: Anal. Calc. for C27H10N2O17Ru5S5: C, 24.95; H, 0.78; N, 2.15. Found: C, 25.28; H, 0.85; N, 2.24%. IR (nuCO, CH2Cl2): 2124s, 2093s, 2066vs, 2041s, 2016s, 1958w cm-1. 1H NMR (CD2Cl2): aromatic region, major isomer, delta 8.13 (d, J 7.2Hz, 1H), 7.93-7.74 (m, 7H); hydride region, major isomer, delta-13.67 (d, J 2.0Hz, 1H),-15.55 (d, J 2.0Hz, 1H), minor isomer, delta-13.78 (d, J 2.0Hz, 1H),-16.07 (d, J 2.0Hz, 1H). Major/minor=21:1. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
17% | In cyclohexane; at 81℃; for 0.5h;Inert atmosphere; Schlenk technique; | TsacH (63mg, 0.32mmol) was added to a cyclohexane solution (20mL) of [Ru3(CO)12] (100mg, 0.16mmol) and the reaction mixture was heated to reflux for 30min. The reaction mixture was then allowed to cool at room temperature. The solvent was removed under reduced pressure and the residue separated by TLC on silica gel. Elution with n-hexane/CH2Cl2 (v/v, 1:1) developed a yellow-orange band corresponding to [HRu5(CO)15(mu-N,S-tsac)(mu5-S)] (5). The product was recrystallized from n-hexane/CH2Cl2 at 4C to afford 5 as red crystals (18mg, 17%). Data for 5: Anal. Calc. for C22H5NO17Ru5S3: C, 22.84; H, 0.44; N, 1.21. Found: C, 23.14; H, 0.48; N, 1.23%. IR (nuCO, CH2Cl2): 2106w, 2083s, 2071vs, 2034s, 2014s, 1967w cm-1. 1H NMR (CDCl3): delta 7.88 (d, J 7.6Hz, 1H), 7.81 (t, J 7.6Hz, 1H), 7.72 (d, J 7.6Hz, 1H), 7.66 (t, 7.6Hz, 1H),-17.87 (s, 1H). |