27148-03-4, Benzo[d]isothiazole-3(2H)-thione 1,1-dioxide is a isothiazole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
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., 27148-03-4
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Reference£º
Article; Mia, Md. Jadu; Reza, Md. Selim; Bhoumik, Nikhil C.; Ghosh, Shishir; Nesterov, Vladimir N.; Richmond, Michael G.; Kabir, Shariff E.; Journal of Organometallic Chemistry; vol. 906; (2020);,
Isothiazole – Wikipedia
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