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Prepht xdb c18 column

Manufactured by Agilent Technologies
Sourced in United States

The PrepHT XDB-C18 column is a preparative high-performance liquid chromatography (HPLC) column designed for the purification and separation of a wide range of compounds. The column features a silica-based C18 stationary phase that provides excellent retention and selectivity for a variety of sample types. The column's dimensions and packing material are optimized for preparative-scale separations, allowing for efficient and high-throughput purification of target analytes.

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3 protocols using prepht xdb c18 column

1

Analytical Techniques for Compound Characterization

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Optical rotations were measured using a Perkin Elmer 341 Polarimeter. IR spectra were taken on a Shimadzu FTIR-8400S infrared spectrophotometer. Ultraviolet (UV) spectra were recorded on a Kontron Uvikon 9X3W Double Beam UV/Vis spectrophotometer (Bioserv, France). Mass spectra were recorded with a Bruker maxis II Electron Transfer Dissociation (ETD). For the collision-induced dissociation (CID) spectra, the collision energy was 40 eV and the collision gas was nitrogen. The NMR experiments were recorded on Bruker Avance III HD 300 MHz, 400 MHz, 500 MHz and 600 MHz spectrometers (Wissembourg, France) equipped with a BBFO Plus Smartprobe and a triple resonance TCI cryoprobe, respectively. Chemical shifts are expressed in δ (ppm), and are referenced to the residual non-deuterated solvent signals. Preparative High-Performance Liquid Chromatography (HPLC) was performed on an Agilent system (Technologies 1260 infinity) and an Agilent PrepHT XDB-C18 column (21.2 × 150 mm i.d.; 5 µm; USA). Column chromatography (CC) was performed using silica gel (Geduran Si 60, 40−63 µm, Merck, Germany and Lichroprep RP-18, 40−63 µm, Merck KGaA, Germany) and Sephadex LH-20 (Sigma-Aldrich Lipophilic Sephadex, Germany). Silica gel-precoated plates (F254, 20 × 20 cm, Merck KGaA, Germany) were used for thin-layer chromatography (TLC).
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2

Synthesis and Purification of Bioactive Compounds

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Lenalidomide (1) was purchased from AstaTech and used as received. VHL ligand (26) was purchased from Abosyn and used as received. GMP and GDP were purchased from ChemImpex and used as received. All solvents and reagents were used without further purification. Yields refer to chromatographically and spectroscopically (1H NMR) homogeneous materials, unless otherwise stated. Reactions were monitored by thin-layer chromatography (TLC) carried out on 0.25-mm SiliCycle silica gel plates (60F-254) using UV-light (254 nm). Flash chromatography was performed using SiliaFlash P60 silica gel. Analytical RP-HPLC was performed using an Agilent 1260 Infinity HPLC equipped with a ZORBAX Eclipse XDB-C18 column (4.6 × 150 mm; 5 μm) at a flow rate of 1 mL/min, with detection at 214 and 254 nm. Semi-preparative HPLC was carried out on Agilent 1260 Infinity HPLC equipped with a PrepHT XDB-C18 column (21.2 × 150 mm; 5 μm) at a flow rate of 18 mL/min using 95% water as a mobile phase and detection at 254 nm and 214 nm. NMR spectra were performed on a 300 MHz Bruker instrument and calibrated using a solvent peak as an internal reference. Spectra were processed using MestReNova software. Mass spectrometry (HRMS) was performed using an Agilent 6520 Accurate-Mass Q-TOF LC/MS spectrometer using ESI ionization with less than 5-ppm error for all HRMS analyses.
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3

Guttiferones A and C Purification

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Guttiferones A (1) and C (6) were obtained as described. 24 Trifluoroacetic acid and formic acid were of reagent grade from Fluka. Gradient grade HiPersSolv acetonitrile from VWR was used. HPLC analysis was performed on Gilson system (pump 305, pump 306, gradient dynamic mixer 811B and autoinjector 234) with an Agilent C18 column (21.2x150 mm, 5 µm). The system was controlled and the results were analysed by Unipoint Gilson software. Column was eluted with an appropriate solvent system at a flow of 1.0 mL/min: (solvent A: water, 0.1% trifluoroacetic acid; solvent B: 50% water/50% acetonitrile, 0.1% trifluoroacetic acid) 0-5 min (isocratic 90/10), 5-8 min (gradient up to 50/50), 8-15 min (gradient up to 20/80), 15-20 min (isocratic 20/80). The detection was at 240 nm. Preparative HPLC was performed on an Agilent system, using an Agilent PrepHT XDB-C18 column (21.2 x 150 mm; 5 μm; USA). Sample was injected and separated using the same gradient program for HPLC analysis (gradient 45 mL/min). Optical rotations were measured with a Perkin-Elmer 341 polarimeter. HRMS measurements were performed on a Waters QTOF I mass instrument. 1D and 2D NMR spectra were monitored on a Brucker NMR 400 MHz and 100 MHz instruments using CD3OD ( H 3.31 and  C 49.0) as solvent. Chemical shifts (δ) are reported in parts per million (ppm), and coupling constants (J) are given in hertz (Hz).
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