All commercial reagents and solvents were used as provided. Flash chromatography was performed with Ultrapure silica gel or with RediSep Rf silica gel columns on a Teledyne ISCO CombiFlash Rf system using the solvents as indicated. Reverse-phase chromatography was performed with C18-bound silica gel. The general method for purification of these compounds involved the adjustment of the pH of aqueous TFA salt solutions to 8.0 using 28% aqueous ammonia, followed by evaporation. The residues were loaded on a C-18 bound silica gel cartridge, followed by elution with water. Relevant fractions were lyophilized to obtain the final compounds. Nuclear magnetic resonance (NMR) spectra were recorded on a Varian 600 MHz (Agilent Technologies, Santa Clara, CA) or Bruker 400 spectrometer (Bruker, Billerica, MA) with Me4Si or signals from the residual solvent as the internal standard for 1H and 13C. Chemical shifts are reported in ppm, and signals are described as s (singlet), d (doublet), t (triplet), q (quartet), m (multiplet), brs (broad singlet), and dd (double doublet). Values given for coupling constants are first order. High-resolution and low-resolution mass spectra were recorded on an Agilent TOF II TOF/MS instrument equipped with an ESI interface. All compounds were >95% pure by HPLC analysis.
Varian 600 mhz
Manufactured by Agilent Technologies
Sourced in United States
The Varian 600 MHz is a high-resolution nuclear magnetic resonance (NMR) spectrometer designed for advanced analytical applications. It provides a magnetic field strength of 600 MHz, enabling the acquisition of high-quality data for the structural elucidation and identification of chemical compounds.
Automatically generated - may contain errors
Lab products found in correlation
400 spectrometer, by Bruker (3 mentions)
Agilent 6230 lc tof ms spectrometer, by Agilent Technologies (2 mentions)
Combiflash rf 200, by Teledyne (2 mentions)
Isco combiflash rf system, by Teledyne (1 mentions)
Tof 2 tof ms instrument, by Agilent Technologies (1 mentions)
Redisep column, by Teledyne (1 mentions)
Agilent 1260 infinity hplc, by Agilent Technologies (1 mentions)
3 protocols using varian 600 mhz
1
Purification and Characterization of Compounds
2
Synthesis and Characterization of PF74
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All commercial chemicals were used as supplied unless indicated otherwise. Compounds were purified via flash chromatography using a Combiflash RF-200 (Teledyne ISCO, Lincoln, NE, USA) with RediSep columns (silica) and indicated mobile phase. 1H and 13C NMR spectra were recorded on a Varian 600 MHz (Agilent Technologies, Santa Clara, CA, USA) or Bruker 400 spectrometer (Bruker, Billerica, MA, USA). Diastereomeric ratio was determined by 1H NMR analysis. Mass data were acquired using an Agilent 6230 TOF LC/MS spectrometer (Agilent Technologies). PF74 was synthesized according to reported procedures43 ,44 (link).
3
Synthetic Protocols for Purified Compounds
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All commercial chemicals were used as supplied unless indicated otherwise. Compounds were purified via flash chromatography using a Combiflash RF-200 (Teledyne ISCO, Lincoln, NE, USA) with RediSep columns (Teledyne ISCO, Lincoln, NE, USA) (silica) and indicated mobile phase. 1H and 13C NMR spectra were recorded on a Varian 600 MHz (Agilent Technologies, Santa Clara, CA, USA) or Bruker 400 spectrometer (Bruker, Billerica, MA, USA). Diastereomeric ratio was determined by 1H NMR analysis. Mass data were acquired using an Agilent 6230 TOF LC/MS spectrometer (Agilent Technologies, Santa Clara, CA, USA). Compound purity analysis was performed using Agilent 1260 Infinity HPLC (Agilent Technologies, Santa Clara, CA, USA) with an Eclipse C18 column (3.5 μm, 4.6 × 100 mm). HPLC conditions: flow rate, 1.0 mL/min; solvent A, 0.1% TFA in water; solvent B, 0.1% TFA in acetonitrile; gradient (B, %): 0–3 min (5–100), 3–11 min (100), 11–13 min (100–5). Determined purity was >85% for all final compounds.
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