UV spectra were recorded on a Milton Roy Spectronic 300 Array spectrophotometer (Rochester, Monroe, NY, USA), and IR spectra were obtained on a Perkin-Elmer FT-IR 1760X spectrophotometer (Norwalk, Fairfield, CT, USA). Optical rotation was measured on a Perkin-Elmer 341 polarimeter (Norwalk, Fairfield, CT, USA). Mass spectra were recorded on a Bruker micro TOF mass spectrometer (ESI-QqTOF-MS) (Manchester, UK). NMR spectra were recorded on a Bruker Avance DPX-300 FT-NMR spectrometer or a Bruker Avance III HD 500 NMR spectrometer (Rheinstetten, Germany). Column chromatography (CC) was performed on silica gel 60 (Kieselgel 60, 70–320 µm, Merck, Darmstadt, Germany), silica gel 60 (Kieselgel 60, 230–400 µm, Merck, Darmstadt, Germany), C-18 (Kieselgel 60 RP-18, 40–63 µm, Merck, Darmstadt, Germany), Diaion HP (Mitsubishi Chemical, Tokyo, Japan) and Sephadex LH-20 (25–100 µm, GE Healthcare, Göteborg, Sweden).
Kieselgel 60 rp 18
Manufactured by Merck Group
Sourced in Germany
Kieselgel 60 RP-18 is a silica-based reversed-phase chromatography material used for the separation and purification of various organic compounds. It consists of silica gel particles with chemically bonded octadecylsilane (C18) functional groups.
Automatically generated - may contain errors
Lab products found in correlation
Kieselgel 60, by Merck Group (3 mentions)
341 polarimeter, by PerkinElmer (1 mentions)
Spectronic 300 array spectrophotometer, by PerkinElmer (1 mentions)
Ft ir 1760x spectrophotometer, by PerkinElmer (1 mentions)
Microtof mass spectrometer, by Bruker (1 mentions)
Avance dpx 300 ft nmr spectrometer, by Bruker (1 mentions)
Avance 3 hd 500 nmr spectrometer, by Bruker (1 mentions)
Sephadex lh 20, by GE Healthcare (1 mentions)
J 815 cd, by Jasco (1 mentions)
I proh, by ITW Reagents (1 mentions)
Chcl3, by ITW Reagents (1 mentions)
Ch2cl2, by ITW Reagents (1 mentions)
P 1010 digital, by Jasco (1 mentions)
6120 quadrupole lc ms instrument, by Agilent Technologies (1 mentions)
Kieselgel 60 f254, by Merck Group (1 mentions)
3 protocols using kieselgel 60 rp 18
1
Spectroscopic and Chromatographic Techniques
2
Analytical and Preparative TLC of Natural Compounds
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Analytical and preparative TLCs were carried out on silica gel (Merck, Kieselgel 60, F254, 0.25, and 0.5 mm) and reverse phase (Merck, Kieselgel 60 RP-18, F254, 0.20 mm) plates. The spots were visualized by exposure to UV radiation (254 and/or 312 nm) or by spraying first with 10% H2SO4 in MeOH, and then with 5% phosphomolybdic acid in EtOH, followed by heating at 110 °C for 10 min on a hot plate. Column chromatography was performed using silica gel (Merck, Kieselgel 60, 0.063–0.200 mm). Solvents n-hexane MeOH, i-PrOH, CHCl3, and CH2Cl2 were purchased from Panreac AppliChem (Barcelona, Spain). Unless otherwise noted, optical rotation was measured in MeOH on a Jasco (Tokyo, Japan) polarimeter, whereas the CD spectrum was recorded on a JASCO J-815 CD in MeOH. 1H and 13C NMR and 2D NMR spectra were recorded at 400 or 500, and 100 or 125 MHz in CDCl3 on Bruker and Varian instruments. The same solvent was used as an internal standard. HR-ESIMS analyses were performed using the LC/MS TOF system (AGILENT 6230B, HPLC 1260 Infinity) column Phenomenex LUNA (C18 (2) 5 µm 150 × 4.6 mm). 1H-NMR and ESI/MS (+) spectra of the identified compounds are reported in the Supplementary Figures S1–S14 .
3
Characterization of Chemical Compounds
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Optical rotations were measured in MeOH on a P-1010 digital polarimeter (Jasco, Tokyo, Japan), unless otherwise noted. IR spectra were recorded as a glass film deposits using a 5700 FT-IR spectrometer (Jasco), and UV spectra were measured in MeCN on a V-530 spectrophotometer (Easton). 1 H and 13 C NMR spectra were recorded, respectively, at 400 and 100 MHz in CDCl 3 , on a Bruker spectrometer (Billerica), using the same solvent as internal standard. The multiplicities were determined by DEPT spectrum (Berger and Braun, 2004) . COSY, HSQC, HMBC and NOESY spectra were recorded using Bruker microprograms. HR ESIMS spectra were recorded on a 6120 Quadrupole LC/MS instrument (Agilent Technologies). Analytical (0.25 mm thickness) and preparative TLC (0.50 mm thickness) were performed on silica gel (Kieselgel 60, F 254 ,) and on reversed phase (Kieselgel 60 RP-18, F 254 , 0.20 mm tickness) plates (Merck). Resulting spots were visualized by exposure to UV radiation (253 nm), or by spraying first with 10% H 2 SO 4 in MeOH and then with 5% phosphomolybdic acid in EtOH, followed by heating at 110°C for 10 min. Column chromatography was performed using silica gel (Merck, Kieselgel 60, 0.063-0.200 mm).
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