Agilent 6210 time of flight lc ms system

All commercially available reagents, compounds, and solvents were purchased and used without further purification. Column chromatography on silica gel was performed on RediSep column using the Teledyne Isco CombiFlash Rf system. Preparative purification was performed on a Waters semi-preparative HPLC. The column used was a Phenomenex Luna C18 (5 micron, 30 × 75 mm) at a flow rate of 45 mL/min. The mobile phase consisted of acetonitrile and water (each containing 0.1% trifluoroacetic acid). A gradient of 10% to 50% acetonitrile over 8 minutes was used during the purification. Fraction collection was triggered by UV detection (220 nm).
¹H spectra were recorded using an INOVA 400 MHz spectrometer (Varian). Samples were analyzed on an Agilent 1200 series LC/MS using a Zorbax Eclipse XDB-C18 reverse phase (5 micron, 4.6 × 150 mm) column and a flow rate of 1.1 mL/min. The mobile phase was a mixture of acetonitrile and H₂O each containing 0.05% trifluoroacetic acid. LC Method A: a gradient of 4% to 100% acetonitrile over 7 minutes was used during analytical analysis. LC Method B: a gradient of 4% to 100% acetonitrile over 3 minutes was used during analytical analysis. High resolution mass spectrometry was recorded on Agilent 6210 Time-of-Flight LC/MS system. Spectra of compounds are listed in Supplementary File 18.

All commercially available reagents, compounds, and solvents were purchased and used without further purification. Column chromatography on silica gel was performed on RediSep column using the Teledyne Isco CombiFlash Rf system. Preparative purification was performed on a Waters semi-preparative HPLC. The column used was a Phenomenex Luna C18 (5 micron, 30 × 75 mm) at a flow rate of 45 mL/min. The mobile phase consisted of acetonitrile and water (each containing 0.1% trifluoroacetic acid). A gradient of 10% to 50% acetonitrile over 8 minutes was used during the purification. Fraction collection was triggered by UV detection (220 nm).
¹H spectra were recorded using an INOVA 400 MHz spectrometer (Varian). Samples were analyzed on an Agilent 1200 series LC/MS using a Zorbax Eclipse XDB-C18 reverse phase (5 micron, 4.6 × 150 mm) column and a flow rate of 1.1 mL/min. The mobile phase was a mixture of acetonitrile and H₂O each containing 0.05% trifluoroacetic acid. LC Method A, a gradient of 4% to 100% acetonitrile over 7 minutes was used during analytical analysis. LC Method B, a gradient of 4% to 100% acetonitrile over 3 minutes was used during analytical analysis. High resolution mass spectrometry was recorded on Agilent 6210 Time-of-Flight LC/MS system.