Kieselgel si 60

1D and 2D NMR spectra were recorded on a Bruker DRX 400 (Bruker BioSpin GmbH, Rheinstetten, Germany) spectrometer, using standard Bruker pulse sequences. Chemical shifts internally referenced to residual solvent signals are given on a δ (ppm) scale. Column chromatography separations were performed with Kieselgel Si 60 (Merck, Darmstadt, Germany). HPLC separations were conducted on a CECIL 1100 Series liquid chromatography pump (Cecil Instruments Ltd., Cambridge, UK) equipped with a GBC LC-1240 refractive index detector (GBC Scientific Equipment, Braeside, VIC, Australia), using a Kromasil 100-7-C₁₈ (250 × 10 mm, Akzonobel, Eka Chemicals AB, Separation Products, Bohus, Sweden) for reversed-phase HPLC or a 250 mm × 10 mm i.d. Kromasil 100-10-SIL (Akzonobel, Eka Chemicals AB, Separation Products, Bohus, Sweden) for normal-phase HPLC. TLC was performed on Kieselgel 60 F₂₅₄ (0.2 mm) precoated aluminum or glass plates (Merck, Darmstadt, Germany), and spots were visualized after spraying with H₂SO₄ in MeOH (20% v/v) reagent and heating at 100 °C for 1 min.

Chromatography experiments were performed on 100 × 100 mm glass plates percolated with a 0.25 mm layer of silica-HPTLC Kieselgel Si 60 with a fluorescent indicator (Merck, Darmstad, Germany). Before use, the plates were washed with methanol and acetone and dried for five minutes at 105 °C for activation. During the experiments, the plates were developed in horizontal Teflon DS chambers (Chromdes, Lublin, Poland). The distance was 90 mm. Before the development, the plates were conditioned for 15 min above the mobile phase. All the solvents used in the planar chromatography experiments were of pro-analytical grade and were purchased from Polish Reagents (POCh, Gliwice, Poland). Techniques of isocratic elution and MGD (multiple gradient development) techniques were used. In the MGD technique, the plate was developed several times (2–9 times). The migration of the mobile phase was dependent on the composition of eluents—the elution strength of the mobile phase was adjusted to the type of the sample [79 (link)]. After each development step, the eluent was evaporated from the chromatographic plates.

1D and 2D NMR spectra were recorded on Bruker DRX 400 (Bruker BioSpin GmbH, Rheinstetten, Germany) and Varian 300 and Varian 600 (Varian, Inc., Palo Alto, CA, USA) spectrometers, using standard Bruker or Varian pulse sequences. Chemical shifts internally referenced to residual solvent signals are given on a δ (ppm) scale. High-resolution ESI and APCI mass spectra were measured on a Thermo Scientific LTQ Orbitrap Velos mass spectrometer (ThermoFisher Scientific, Bremen, Germany). Column chromatography separations were performed with Kieselgel Si 60 (Merck, Darmstadt, Germany). HPLC separations were conducted on a CECIL 1100 Series liquid chromatography pump (Cecil Instruments Ltd., Cambridge, UK) equipped with a GBC LC-1240 refractive index detector (GBC Scientific Equipment, Braeside, VIC, Australia), using a 250 mm × 22 mm i.d. Techsil 10 ODS column (Wellington House, Cheshire, UK) for reversed-phase HPLC or a 250 mm × 10 mm i.d. Kromasil 100-10-SIL (Akzonobel, Eka Chemicals AB, Separation Products, Bohus, Sweden) for normal-phase HPLC. TLC was performed on Kieselgel 60 F₂₅₄ (0.2 mm) precoated aluminum or glass plates (Merck, Darmstadt, Germany), and spots were visualized after spraying with H₂SO₄ in MeOH (20% v/v) reagent and heating at 100 °C for 1 min.