Kieselgel 60 f254 aluminum plates

Optical rotations were measured on a Krüss polarimeter (A. KRÜSS Optronic GmbH, Hamburg, Germany) equipped with a 0.5 dm cell. UV spectra were recorded on a Lambda 40 UV/Vis spectrophotometer (Perkin Elmer Ltd., Beaconsfield, UK). IR spectra were obtained on an Alpha II FTIR spectrometer (Bruker Optik GmbH, Ettlingen, Germany). Low-resolution EI mass spectra were measured on a Thermo Electron Corporation DSQ mass spectrometer (Thermo Electron Corporation, Austin, TX, USA) using a Direct-Exposure Probe (Thermo Electron Corporation, Austin, TX, USA). NMR spectra were recorded on a DRX 400 spectrometer (Bruker BioSpin GmbH, Rheinstetten, Germany). The 2D experiments (HSQC, HMBC, COSY, NOESY) were performed using standard Bruker pulse sequences. Column chromatography separations were performed with Kieselgel 60 (Merck, Darmstadt, Germany). HPLC separations were conducted on a Pharmacia LKB 2248 liquid chromatography pump (Pharmacia LKB Biotechnology, Uppsala, Sweden) equipped with a RI-102 Shodex refractive index detector (ECOM spol. s r.o., Prague, Czech Republic) using an Econosphere Silica 10 μm (250 × 10 mm i.d.; Grace, Columbia, MD, USA) column. TLC were performed with Kieselgel 60 F₂₅₄ aluminum plates (Merck, Darmstadt, Germany) and spots were detected after spraying with 20% H₂SO₄ in MeOH reagent and heating at 100 °C for 1 min.

Optical rotations were measured on a Krüss polarimeter (A. KRÜSS Optronic GmbH, Hamburg, Germany) equipped with a 0.5 dm cell. UV spectra were recorded on a Lambda 40 UV/Vis spectrophotometer (Perkin Elmer Ltd., Beaconsfield, UK). IR spectra were obtained on a Alpha II FTIR spectrometer (Bruker Optik GmbH, Ettlingen, Germany). High-resolution APCI mass spectra were measured on a LTQ Orbitrap Velos mass spectrometer (Thermo Fisher Scientific, Bremen, Germany). NMR spectra were recorded on Avance NEO 950, Avance NEO 700, Avance III 600, and DRX 400 spectrometers (Bruker BioSpin GmbH, Rheinstetten, Germany). Chemical shifts are given on a δ (ppm) scale using TMS as internal standard. The 2D experiments (HSQC, HMBC, COSY, NOESY) were performed using standard Bruker pulse sequences. Column chromatography separations were performed with Kieselgel 60 (Merck, Darmstadt, Germany). HPLC separations were conducted using a Waters 600 liquid chromatography pump equipped with a Waters 410 differential refractometer (Waters Corporation, Milford, MA, USA), using a 25 cm × 10 mm Econosphere Silica 10 μ column (Grace, Columbia, MD, USA). TLC were performed with Kieselgel 60 F₂₅₄ aluminum plates (Merck, Darmstadt, Germany) and spots were detected after spraying with 20% H₂SO₄ in MeOH reagent and heating at 100 °C for 1 min.