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2 protocols using sil g uv254 0.20 mm

1

Spectroscopic Characterization of Organic Compounds

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IR spectra were recorded on a JASCO FT-IR (4100) spectrometer. High-resolution mass determination was carried out using a Finnigan TSQ quantum ultra mass spectrometer (Thermo Scientific). NMR spectra were recorded at 300 K on Bruker Avance III spectrometers with chloroform-d1 as solvent and internal standard. The solvent signal was referenced to δH 7.24 ppm and δC 77.0 ppm, respectively. Analytical HPLC was performed on an Agilent 1100 Series LC/MSD trap. Flash column chromatography was undertaken using silica gel 60 M (230–400 mesh). TLC analyses were performed on silica gel plates (Sil G/UV254 0.20 mm, Macherey-Nagel) using a 9:1 mixture of chloroform and methanol as the eluent. Analytes were detected with vanillin-sulfuric acid spray reagent.
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2

Spectroscopic Characterization of Compounds

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Optical rotation was measured with a JASCO P-1020 polarimeter at 25 °C (JASCO, Gross-Umstadt, Germany). UV spectra were recorded on a Shimadzu UV-1800 spectrophotometer (Shimadzu, Kyoto, Japan) and IR spectra on a JASCO FT-IR (4100) spectrometer. 1 H and 13 C NMR, DEPT and 2D NMR spectra were measured on Bruker Avance III 500 MHz and Bruker Avance III 600 MHz (equipped with a Bruker Cryo Platform) instruments (Bruker, Fällanden, Switzerland). The chemical shift values (δ) are given in ppm and coupling constants in Hz. 1 H and 13 C chemical shifts were referenced to the solvent residual peaks for DMSO-d 6 at δ H 2.49 and δ C 39.5, respectively. HRESIMS experiments were carried out on a Thermo Accela UPLC-system combined with a Thermo Exactive mass spectrometer equipped with an electrospray ion source (Thermo Fisher Scientific, Bremen, Germany). Analytical HPLC was performed on an Agilent 1100 Series LC/MSD trap (Agilent Technologies, Santa Clara, CA, USA). Column chromatography was undertaken using silica gel 60 M (230-400 mesh) or Sephadex LH-20 (Pharmacia Biotech AB, Uppsala, Sweden). TLC analyses were performed on silica gel plates (Sil G/UV254 0.20 mm, Macherey-Nagel, Düren, Germany). All solvents used for chromatography, [α] D , UV and MS were HPLC grade.
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