Ac 300 spectrometer

MALDI-OF spectra were performed with a Perspective Biosystems Voyager DE-STR at the I.C.S.N. (CNRS of Gif-sur-Yvette). ¹H-NMR spectra were recorded on Bruker AC-300 spectrometer (300 MHz) with CDCl₃ as reference solvent.

The Infrared (IR) spectra were generated in a Thermo Scientific USA (Nicolet iS50 model) IR spectrometer (Thermo Scientific, Wilmington, DE, USA), coupled to Pike Gladi ATR technologies. Nuclear Magnetic Resonance (NMR) spectra of ¹H and ¹³C were obtained on a Bruker AC-300 spectrometer (Bruker, Billerica, MA, USA) operating at 300 MHz for ¹H NMR and 75 MHz for ¹³C NMR. The samples were solubilized in deuterated methanol or pyridine using tetramethylsilane as the internal reference. Mass spectrometric analyses were performed in a Bruker Compass mass spectrometer by electrospray ionization (range of m/z of 80–1000). The purity of all synthetic compounds was determined by High-Performance Liquid Chromatography (HPLC) using Shimadzu equipment. Thin-layer chromatography experiments were performed on silica gel sheets 60 F254 (Merck, Darmstadt, Germany), and purification by chromatography column was performed on flash silica gel (Sigma-Aldrich, Saint Louis, MO, USA, 220–440 mesh, 0.035 mm–0.075 mm). The visualization of the substances in TLC experiments was performed by using an iodochloroplatinate reagent or in a UV chamber (λ = 254 or 365 nm). Melting points were measured without correction using Mars equipment (PFM II) with a crushed sample packaged in a capillary tube.

¹H NMR and ¹³C NMR analyses were performed at 25 °C on a Bruker AC 300 spectrometer at 300 MHz and 75 MHz, respectively, using chloroform-d as the solvent and tetramethylsilane as the internal standard. HPLC analyses were conducted by an Agilent Technologies 1200 series liquid chromatograph provided with a G1379B degasser, a G1312A pump, and a G1329A autosampler. Separations were attained by means of a Discovery C-18 column (3 μm particle size; 150 mm length; 4.6 mm i.d., Merck KGaA, Darmstadt, Germany). MS/MS spectra were recorded by using an API 4000 Q-Trap (AB Sciex, Framingham, MA, USA) mass spectrometer. Detailed instrumental conditions have been previously reported [24 (link)].

All commercial reagents and solvents were used without further purification. Melting points were determined with an Electrothermal (BI 9300) capillary melting point apparatus (Thermo Fisher Scientific, Waltham, MA) and are uncorrected. The ¹H- and ¹³C-NMR spectra were recorded on an AC300 spectrometer (Bruker, Billerica, MA) at 300 and 75.5 MHz respectively using tetramethylsilane (TMS) as internal standard and CDCl₃ as solvent. Mass spectra were recorded with a LCMS-MS triple-quadrupole system (1200ws, Varian, Palo Alto, CA). Thin layer chromatography (TLC) was carried out on aluminium-baked silica gel 60 (Macherey-Nagel, Hoerdt, France). Column chromatography was performed on silica gel (230–400 mesh). Elemental analyses were performed with a vario MICRO analyser (Elementar, Lyon, France).