All reactions were performed in glassware under a positive pressure of argon. Flash column chromatography was performed on a Teledyne ISCO CombiFlash Rf 200 system (Isco, Inc., Lincoln, NE, USA) using silica gel 60 (230–400 mesh). Thin layer chromatography (TLC) analyses were performed on EMD 250 μm Silica Gel 60 F254 plates (Merck KGaA, Darmstadt, Germany) and visualized by quenching of UV fluorescence (λmax = 254 nm) or by staining with ceric ammonium molybdate. 1H-NMR spectra were recorded on a Varian Inova-400 instrument (Varian, Inc., Palo Alto, CA, USA). Chemical shifts are reported in ppm (δ) relative to the residual solvent signals of the solvent (δ 7.26 for CHCl3), coupling constants (J) are reported in Hz and the multiplicities are presented as follows: s = singlet, brs = broad singlet, d = doublet, t = triplet, q = quartet, and m = multiplet. Mass spectra were acquired on Agilent 6120 Single Quadrupole Liquid Chromatography tandem Mass Spectrometer (LC/MS) (Agilent Technologies, Santa Clara, CA, USA). High-resolution mass spectrum was acquired by the Mass Spectrometry Facility at the University of Austin.
Combiflash rf 200 system
Manufactured by Teledyne
Sourced in United States
The CombiFlash Rf 200 system is a flash chromatography instrument designed for automated purification of chemical compounds. It provides precise control of flow rate, gradient, and fraction collection to facilitate efficient separation and purification of sample mixtures.
Automatically generated - may contain errors
Lab products found in correlation
Emd 250 μm silica gel 60 f254 plates, by Merck Group (2 mentions)
Agilent 6120 single quadrupole liquid chromatography tandem mass spectrometer lc ms, by Agilent Technologies (2 mentions)
Inova 400 instrument, by Agilent Technologies (2 mentions)
Imatinib, by Merck Group (1 mentions)
Spectrum one, by PerkinElmer (1 mentions)
400 mhz spectrometer, by Agilent Technologies (1 mentions)
Silica gel 60 f254 plate, by Merck Group (1 mentions)
Mp90 melting point apparatus, by Mettler Toledo (1 mentions)
Avance 3 500, by Bruker (1 mentions)
6 protocols using combiflash rf 200 system
1
Purification and Characterization of Organic Compounds
2
Purification and Characterization of Organic Compounds
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All reactions were performed in glassware under a positive pressure of argon. Flash column chromatography was performed on a Teledyne ISCO CombiFlash Rf 200 system (Isco, Inc., Lincoln, NE, USA) using silica gel 60 (230–400 mesh). Thin layer chromatography (TLC) analyses were performed on EMD 250 μm Silica Gel 60 F254 plates (Merck KGaA, Darmstadt, Germany) and visualized by quenching of UV fluorescence (λmax = 254 nm) or by staining with ceric ammonium molybdate. 1H-NMR spectra were recorded on a Varian Inova-400 instrument (Varian, Inc., Palo Alto, CA, USA). Chemical shifts are reported in ppm (δ) relative to the residual solvent signals of the solvent (δ 7.26 for CHCl3), coupling constants (J) are reported in Hz and the multiplicities are presented as follows: s = singlet, brs = broad singlet, d = doublet, t = triplet, q = quartet, and m = multiplet. Mass spectra were acquired on Agilent 6120 Single Quadrupole Liquid Chromatography tandem Mass Spectrometer (LC/MS) (Agilent Technologies, Santa Clara, CA, USA). High-resolution mass spectrum was acquired by the Mass Spectrometry Facility at the University of Austin.
3
Synthesis and Characterization of Organic Compounds
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All chemicals used were purchased from Merck and Aldrich without further purification. Trimetazidine HCl was obtained from the World Medicine Drug Company (Fisher Scientific), Imatinib was purchased from Sigma Aldrich (SML1027-100MG). Sonication was performed in an Intersonik ultrasound cleaner (model: MIN4) with a frequency of 25 kHz, an US output power of 100 W, a heating 200 W. Heidolph RV Laborata 4000 rotary evaporator was used to evaporate the solvent. A TLC Merck 5554 with silica gel layers with fluorescent indicator and a Camag (254/366 nm) UV lamp were used. The melting points of the pure materials were measured on the Stuart apparatus. FTIR spectra of the starting materials and the obtained products were taken on a “Perkin Elmer Spectrum One” FTIR spectrometer by ATR technique. 1H and 13C NMR spectra were obtained from a “Bruker 500 MHz” spectrometer in CDCl3. Chemical shifts were reported in ppm (parts per million) with respect to internal standard TMS (Tetramethylsilane). LC-MS spectra were obtained by Agilient 6200 series TOF/6500 series TOF/Q-TOF Mass Spectrometer. All crude products were purified with Teledyne Isco CombiFlash Rf 200 system and RediSep Rf Gold Silica Columns.
4
Isolation and Purification of Compound 1 from Marine Actinomycete
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R818 spores from Marine Agar 2216 (MA) plates were inoculated into 60 250-mL flasks; each flask contains 100 mL of SPY media (soluble starch 20 g, glucose 10 g, peptone 5 g, yeast extract 5 g, K2HPO4 0.5 g, MgSO4⋅7H2O 0.5 g, CaCO3 2 g, and sea salt 39.5 g, per liter) supplemented with 2 mM LaCl3. Flasks were incubated on a shaker at 200 rpm and 28°C for 7 days. The broth (6 L) was extracted with four times with an equal volume of EtOAc, and the combined EtOAc layers were concentrated under vacuum. The crude extract (4.9 g) was fractioned on a CombiFlash Rf200 system (Teledyne Isco) using a RediSep Rf Gold C18 column (size 50 g) with a flow rate of 40 mL/min. Fractions with antifungal activity were pooled and used for bioactivity-guided purification. Compound 1 (2.0 mg) was purified by semi-preparative HPLC (H2O+0.1% TFA/MeCN: 70/30, flow rate at 3 mL/min) using an Apollo C18 column (250 mm × 10 mm).
5
Purification and Characterization of Organic Compounds
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All commercially available chemicals were of reagent grade and were used without further purification. Solvents were dried with standard procedures. All of the reactions were purified by flash column chromatography using CombiFlash® Rf 200 system (Teledyne Isco., Lincoln, NE). Additionally, thin-layer chromatography was performed on 0.25 mm silica gel 60-F254 plates (Merck, Kenilworth, NJ). Visualisation was accomplished with 254 nm of UV light or potassium permanganate staining followed by heating. The proton nuclear magnetic resonance (1H-NMR) spectra were determined on a Varian (400 and 100 MHz) or Bruker (400 and 100 MHz). 1H NMR (at 400 MHz) was reported on a Varian 400 MHz spectrometer and are reported in ppm using solvent as an internal standard (DMSO-d6 at 2.50, Acetone-d6 at 2.05, at 3.31 for 1H NMR). Data reported as (s = singlet, d = doublet, t = triplet, q = quartette, m = multiplet, br = broad; coupling constant(s) in Hz; integration). LC/MS data were obtained using a Waters 2695-ZQ2000 system and Waters ACQUITY UPLC-SQ Detector 2.
6
Characterization of Novel Organic Compounds
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Unless otherwise noted, all commercial reagents and solvents were obtained from the commercial provider and used without further purification. Melting points (mp) were obtained with a MP90 melting point apparatus and were uncorrected (Mettler-Toledo, Greifensee, Switzerland). 1H-NMR and 13C-NMR spectra were recorded on a Bruker Avance III 500 (500 MHz for 1H-NMR; 126 MHz for 13C-NMR) spectrometer (Varian, San Francisco, CA, USA) with Me4Si as the internal standard. ESI high-resolution mass spectra (HRMS) were recorded on an Autospec Ultima-TOF spectrometer (Micromass UK Ltd., Manchester, UK). Flash chromatography was performed on a Combiflash Rf 200 system (Teledyne-Isco, Lincoln, NE, USA).
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