All solvents
and reagents were obtained from commercial sources (Fisher Scientific,
VWR Scientific, Sigma-Aldrich, Combi-Blocks) and used without further
purification, unless otherwise noted. All reactions were performed
under a positive pressure of nitrogen or argon in flame-dried glassware.
Reactions were monitored using glass-backed TLC plates impregnated
with a fluorescent indicator absorbing at 254 nm. Silica gel chromatography
was performed on a CombiFlash Rf Teledyne ISCO system using
hexane, EtOAc, dichloromethane (DCM), or MeOH as eluents. C18 reverse phase chromatography was performed on the same instrument
using 0.1% formic acid in methanol, acetonitrile, or water as an eluent. 1H and 13C NMR spectra were obtained on a Varian
(400 MHz) spectrometer, Jeol (400 MHz) spectrometer, or a VX (500
MHz) equipped with XSens cold probe (Varian) spectrometer in the Department
of Chemistry and Biochemistry at UC San Diego. The purity of all compounds
used in assays and cell studies was determined to be ≥95% by
HPLC analysis. Mass spectrometry was performed at the UC San Diego
Molecular Mass Spectrometry Facility. HRMS analysis was performed
using an Agilent 6230 Accurate-Mass LC-TOFMS located at the UC San
Diego Molecular Mass Spectrometry Facility.
and reagents were obtained from commercial sources (Fisher Scientific,
VWR Scientific, Sigma-Aldrich, Combi-Blocks) and used without further
purification, unless otherwise noted. All reactions were performed
under a positive pressure of nitrogen or argon in flame-dried glassware.
Reactions were monitored using glass-backed TLC plates impregnated
with a fluorescent indicator absorbing at 254 nm. Silica gel chromatography
was performed on a CombiFlash Rf Teledyne ISCO system using
hexane, EtOAc, dichloromethane (DCM), or MeOH as eluents. C18 reverse phase chromatography was performed on the same instrument
using 0.1% formic acid in methanol, acetonitrile, or water as an eluent. 1H and 13C NMR spectra were obtained on a Varian
(400 MHz) spectrometer, Jeol (400 MHz) spectrometer, or a VX (500
MHz) equipped with XSens cold probe (Varian) spectrometer in the Department
of Chemistry and Biochemistry at UC San Diego. The purity of all compounds
used in assays and cell studies was determined to be ≥95% by
HPLC analysis. Mass spectrometry was performed at the UC San Diego
Molecular Mass Spectrometry Facility. HRMS analysis was performed
using an Agilent 6230 Accurate-Mass LC-TOFMS located at the UC San
Diego Molecular Mass Spectrometry Facility.