Mercury 400 100 mhz

All solvents were purified before use. Ethyl acetates were purchased from Acros Organics (Geel, Belgium) and used without purification. Reactions were monitored by thin-layer chromatography (TLC) using Fluka silica gel (60 F 254) plates (0.25 mm). Visualization was performed with UV light. The melting points of the synthesized compounds were taken on a melting point tube. The ¹H NMR spectra were recorded on a Varian Gemini 400 MHz and ¹³C NMR spectra on a Varian Mercury-400 100 MHz in DMSO-d₆ using tetramethylsilane as an internal standard. Chemical shifts are reported in ppm units with use of the d scale. The mass spectra were recorded on an Agilent 1200 LC/MSD SL instrument (Santa Clara, CA, USA).

Reagents were used as purchased without further purification. Solvents (THF, DMF, CH₂Cl₂) were dried and freshly distilled before use according to procedures reported in the literature. Chromatographic separations were performed on silica gel columns by flash (Kieselgel 40, 0.040–0.063; Merck). TLC was performed on precoated silica gel polyester plates (0.25 mm thickness, with UV 254 fluorescent indicator). Melting points were determined on a Buchi 510 apparatus and are uncorrected. ¹H NMR and ¹³C NMR spectra were recorded on a Bruker AC200 spectrometer at 200/50 MHz, on a Bruker SY spectrometer at 400/100 MHz or on a Varian Mercury 400/100 MHz, using CDCl₃ as solvent (unless otherwise stated). Chemical shifts (δ) are given in ppm downfield from tetramethylsilane, and coupling constants (J values) are in Hertz. Electrospray-ionisation (ESI) high-resolution mass spectra (HRMS) were obtained on a VG-TS250 apparatus (70 eV). A Helios Alfa UV-320 from Thermo-Spectronic was used for UV spectra and turbidimetric measurements. IR spectra were acquired in a FTIR Nicolet Impact 410 equipment (film, unless otherwise stated) and the absorptions are expressed in cm⁻¹. The aqueous solubility of the compound was determined in a Helios Alfa Spectrophotometer.