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5 protocols using rp c18 f254s

1

Spectroscopic Analysis of Chemical Compounds

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1D and 2D NMR spectra were obtained on a VARIAN UNITY INOVA 400 spectrometer (Varian, Palo Alto, CA, USA). Mass spectra were determined on a JEOL JMS-AX505WA mass spectrometer (Tokyo, Japan). Column chromatography was carried out over silica gel (40–60 μm, Merck, Kenilworth, NJ, USA) and LiChroprep RP-C18 (40–60 μm, Merck). HPLC (high performance liquid chromatography) was carried out on a Waters 1525 system (Miliford, MA, USA) using reverse-phase column (ODS-2, 5 μm, 4.6 × 15 cm, GL Science, Seoul, Korea). Fractions obtained from column chromatography were monitored by thin layer chromatography (TLC) (RP-C18 F254S and silica gel 60 F254, Merck).
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2

Analytical Characterization of Compounds

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Mass spectra were obtained on a JEOL JMS-AX505WA mass spectrometer. NMR spectra were determined on a Varian UNITY INOVA 400 NMR spectrometer. Column chromatography was carried out over silica gel (40–60 μm, Merck, Kenilworth, NJ, USA). Fractions from column chromatography were monitored by thin layer chromatography (TLC) (silica gel 60 F254 and RP-C18 F254S, Merck) under UV light or by heating after spraying 10% H2SO4 in CH3OH (v/v).
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3

Spectroscopic Characterization of Organic Compounds

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1D and 2D NMR spectra were recorded on an ECZ-400 spectrometer (Jeol Ltd., Tokyo, Japan). The signals of the solution CDCl3 (residual CHCl3 (δH 7.26 ppm) and CDCl3 (δC 77.0 ppm)) were used as internal standards. NMR data were acquired and processed with Delta 6.1.0 or MestReNova v12.2.2 software. MS and HRMS spectra were acquired on an SolariX FTMS mass spectrometer (7 Tesla; Bruker, Bremen, Germany) with an ESI ion source in positive ionization mode. Silica gel (Kieselgel 60, 70–230 or 230–400 mesh, Merck, Darmstadt, Germany), and Sephadex LH-20 gel (Pharmacia Fine Chemicals AB, Uppsala, Sweden) were used for column chromatography (CC). Thin-layer chromatography (TLC) was carried out using silica gel (Kieselgel 60 F254, Merck) and RP-C18 (F254s, Merck) pre-coated plates. For visualization, the compounds were detected on TLC with a developer (50% H2SO4 (v/v) in methanol) followed by heating at 120 °C. HPLC analyses were performed with a pump (model L-2130, Hitachi, Tokyo, Japan) and a diode-array detector (model L-2455, Hitachi, Tokyo, Japan) equipped with an HPLC analytical column (BDS HypersilTM C18, 250 × 4.6 mm, 5 μm, ThermoFisher Scientific Inc., Waltham, MA, USA), and using a mixture of acetonitrile (ACN)/H2O or a mixture of methanol (MeOH)/H2O as the mobile phase (Supplementary Fig. 13).
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4

Analytical Characterization of Compounds

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Mass spectra were obtained using a JEOL JMS-700 mass spectrometer. Nuclear Magnetic Resonance (NMR) spectra were recorded using a Varian UNITY INOVA 400 NMR spectrometer.
Column chromatography was performed using silica gel (4060 μm; Merk, Kenilworth, NJ, USA) and a µ-Bondapak C 18 column (5 μm, 3.9  300 mm; Waters, Milford, MA, USA). Thin layer chromatography (TLC) was performed using Merck precoated silica gel F 254 plates. Spots were detected via TLC (RP-C18 F 254S and silica gel 60 F 254 , Merck) under UV light or by heating after spraying with 10% H 2 SO 4 in CH 3 OH (v/v).
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5

Spectroscopic Analysis of Chemical Compounds

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IR spectra were obtained on a Perkin Elmer Spectrum 100 FT-IR spectrometer. Mass spectra analysis was carried out on Thermo-Scientific TSQ Quantum Access Max LC-MS/MS equipped with an ESI source. High Resolution Mass spectra were obtained on Agilent 6200 Series TOF and 6500 Series QTOF-MS system equipped with an ESI source. Optical rotation measurements were done on a Perkin Elmer Model-351 polarimeter in MeOH at 20 C. 1D and 2D (COSY, HMBC, HSQC and NOESY) NMR spectra were recorded on Varian Oxford AS400 spectrometer with TMS as internal standard at room temperature. 2D NMR spectra were run using standard Varian pulse programs. Column chromatography was carried out on silica gel 60 (40e63 mm-Merck), Sephadex LH-20 (GE Healthcare) and Lichroprep RP-C18 (25e40 mm, Merck) using analytical grade purity solvents (Merck and Sigma). TLC analyses were carried out on silica gel 60 F 254 and RP-C18 F 254s (Merck) pre-coated aluminum plates. Compounds were detected by UV (244e366 nm) and vanillin/H 2 SO 4 reagent followed by heating. Spraying with ninhydrin reagent followed by heating was used to detect the amino acid residue.
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