The reagents were purchased from Merck Life Science S.r.l. and Biosynth
Carbosynth®. Melting points were evaluated on a Buchi
Melting Point B-540 instrument. They are uncorrected and were evaluated on chromatographically purified or recrystallized compounds. The reactions were controlled by thin layer chromatography (TLC), using
Merck silica gel 60 F254 plates preloaded with fluorescent indicator and visualized with UV light (254 nm). Silica gel column (Kieselgel 60) was employed for preparative chromatographic purifications. Na
2SO
4 was used to dry all the solutions which were concentrated with a Buchi
R-114 rotary evaporator at low pressure. Homogeneity of the products was evaluated by analytical reversed-phase HPLC (RP-HPLC) on a Shimadzu-10 ADsp HPLC system by means of a Phenomenex
Kinetex XB-C18 column, 5 μm, 4.6 × 250 mm and applying the gradient of acetonitrile (CH
3CN) in 0.1% aqueous trifluoroacetic acid (TFA), from 0% to 100% in 25 min, at a flow rate of 1 mL/min. Analytical RP-HPLC indicated a purity > 98%.
1H and
13C NMR spectra were recorded on Varian
Mercury Plus 400 MHz instrument in dimethyl sulfoxide (DMSO‑
d6). Chemical shifts are described in ppm, while peak patterns are reported using the abbreviations: m (multiplet), t (triplet), d (doublet), s (singlet). API 2000 Applied Biosystem mass spectrometer was used to determine mass spectra of the final products.
Corvino A., Citi V., Fiorino F., Frecentese F., Magli E., Perissutti E., Santagada V., Calderone V., Martelli A., Gorica E., Brogi S., Colombo F.F., Capello C.N., Araujo Ferreira H.H., Rimoli M.G., Sodano F., Rolando B., Pavese F., Petti A., Muscará M.N., Caliendo G, & Severino B. (2021). H2S donating corticosteroids: Design, synthesis and biological evaluation in a murine model of asthma. Journal of Advanced Research, 35, 267-277.