2525 hplc system

All solvents and reagents were used as obtained. ¹H-NMR spectra were recorded with a Varian Inova 600 NMR spectrometer and referenced to DMSO. Chemical shifts are expressed in ppm. Mass spectra were measured with Waters Micromass ZQ using an ESI source coupled to a Waters 2525 HPLC system operating in reverse mode with a Waters Sunfire C18 5 μm, 4.6 × 50 mm column. Purification of compounds was performed with either a Teledyne ISCO CombiFlash Rf system or a Waters Micromass ZQ preparative system. The purity was analyzed on a Waters LC-MS Symmetry (C18 column, 4.6 × 50 mm, 5 μM) using a gradient of 5%−95% methanol in water containing 0.05% trifluoroacetic acid (TFA). Detailed synthetic schemes and characterization data below (see Scheme 1).

All solvents and reagents were used as obtained. 1H NMR spectra were recorded with a Varian Inova 600 NMR spectrometer and referenced to dimethylsulfoxide. Chemical shifts are expressed in ppm. Mass spectra were measured with Waters Micromass ZQ using an ESI source coupled to a Waters 2525 HPLC system operating in reverse mode with a Waters Sunfire C18 5 µm, 4.6 mm × 50 mm column. Purification of compounds was performed with either a Teledyne ISCO CombiFlash Rf system or a Waters Micromass ZQ preparative system. The purity was analyzed on an above-mentioned Waters LC-MS Symmetry (C18 column,4.6 mm × 50 mm, 5 µM) using a gradient of 5–95% methanol in water containing 0.05% trifluoroacetic acid (TFA). Detailed synthetic schemes and characterization data are presented below and elsewhere.¹

All solvents and reagents were used as obtained. For verification of chemical structures, 1H NMR spectra were recorded with a Varian Inova 500 NMR spectrometer and referenced to dimethyl sulfoxide. Chemical shifts are expressed in ppm. Mass spectra were measured with Waters Micromass ZQ using an ESI source coupled to a Waters 2525 HPLC system operating in reverse mode with a Waters Sunfire C18 5 μm, 4.6 × 50 mm² column. Purification of compounds was performed with either a Teledyne ISCO CombiFlash Rf system or a Waters Micromass ZQ preparative system. The purity was analyzed on an above-mentioned Waters LC—MS Symmetry (C18 column,4.6 × 50 mm², 5 μM) using a gradient of 5–95% methanol in water containing 0.035% trifluoroacetic acid (TFA). Detailed synthetic schemes and characterization data are available in Supplementary Chemical Synthesis Details and else-where.^{5 (link),6 (link)}