General reagents were purchased from Sigma-Aldrich (St. Louis, MO, USA) or ACROS Organics (Belgium). Thin layer chromatography (TLC) was performed on alumina-backed silica gel 40 F254 plates (Merck) and illuminated under UV (254 nm) The melting points were determined on Optimelt MPA100 instrument (SRS, USA) and are uncorrected. Syntheses were performed on a CEM-DISCOVERY microwave reactor (CEM Corporation, Matthews, NC, USA) with temperature and pressure control. High resolution mass spectrometry (HRMS) analysis was performed for all new compounds on SYNAPT G2-S HDMS (Waters, USA). The purity of all compounds was assessed using a Agilent1260 equipped with a DAAD detector at 260 nm, RP-column: Eclipse plus C18 (3,5 μm); flow 0.5 ml/min. The time of each measurement was 21 min. Conditions: 0− 0.8 min (80% H2O (0.1% TFA); 20% acetonitrile); 0.8−7 min (100% acetonitrile); 7−13 min (80% H2O (0.1% TFA); 20% acetonitrile).
All 1H NMR spectra were recorded on a Bruker AM-400 spectrometer (400 MHz) as well as Bruker AVANCE III (500 MHz). Chemical shifts are reported in ppm against the internal standard, Si(CH3)4. Easily exchangeable signals were omitted when diffuse. In general, thiosemicarbazones – 1a, 2a-b, 3a-c, Dp44mT and their thiosemicarbazide precursors were synthesized and characterized, as described previously [35 (link), 36 (link)]. Doxorubicin was purchased from Sigma-Aldrich.
All 1H NMR spectra were recorded on a Bruker AM-400 spectrometer (400 MHz) as well as Bruker AVANCE III (500 MHz). Chemical shifts are reported in ppm against the internal standard, Si(CH3)4. Easily exchangeable signals were omitted when diffuse. In general, thiosemicarbazones – 1a, 2a-b, 3a-c, Dp44mT and their thiosemicarbazide precursors were synthesized and characterized, as described previously [35 (link), 36 (link)]. Doxorubicin was purchased from Sigma-Aldrich.
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