Combiflash companion purification system

¹H NMR spectra were recorded on a Bruker DPX spectrometer at 400 MHz. Chemical shifts are reported as parts per million (ppm) downfield from an internal tetramethylsilane standard or solvent references. For air- and water-sensitive reactions, glassware was flame- or oven-dried prior to use and reactions were performed under argon. Dimethylformamide was dried using the solvent purification system manufactured by Glass Contour, Inc. (Laguna Beach, CA). All other solvents were of ACS chemical grade (Fisher Scientific) and used without further purification unless otherwise indicated. Commercially available starting reagents were used without further purification. Analytical thin-layer chromatography was performed with silica gel 60 F254 glass plates (SiliCycle). Flash column chromatography was conducted self-packed columns containing 200–400 mesh silica gel (SiliCycle) on a Combiflash Companion purification system (Teledyne ISCO). High performance liquid chromatography (HPLC) was performed on a Varian Prostar 210 (Agilent) using Polaris 5 C18-A columns (Analytical: 150 × 4.6 mm, 3 μm; Preparative: 150 × 21.2 mm, 5 μm) (Agilent). Low-resolution mass spectra (LR-MS) were acquired on an Advion Mass-express.

¹H NMR spectra were recorded on a Bruker DPX spectrometer at 400 MHz. Chemical shifts are reported as parts per million (ppm) downfield from an internal tetramethylsilane standard or solvent references. For air- and water-sensitive reactions, glassware was flame- or oven-dried prior to use and reactions were performed under argon. Dimethylformamide was dried using the solvent purification system manufactured by Glass Contour, Inc. (Laguna Beach, CA). All other solvents were of ACS chemical grade (Fisher Scientific) and used without further purification unless otherwise indicated. Commercially available starting reagents were used without further purification. Analytical thin-layer chromatography was performed with silica gel 60 F254 glass plates (SiliCycle). Flash column chromatography was conducted self-packed columns containing 200–400 mesh silica gel (SiliCycle) on a Combiflash Companion purification system (Teledyne ISCO). High performance liquid chromatography (HPLC) was performed on a Varian Prostar 210 (Agilent) using Polaris 5 C18-A columns (Analytical: 150 × 4.6 mm, 3 μm; Preparative: 150 × 21.2 mm, 5 μm) (Agilent). Low-resolution mass spectra (LR-MS) were acquired on an Advion Mass-express.