Sil ht autosampler

All materials and reagents were purchased from Sigma-Aldrich Co. Ltd. and abcr GmbH. All solvents were analytically pure and dried before use. Thin layer chromatography was carried out on aluminum sheets coated with silica gel 60 F254 (Merck, Darmstadt, Germany). For column chromatography under normal pressure silica gel 60 (0.036-0.200 mm) was used.
Final compounds were confirmed to be of >95% purity based on HPLC. Purity was measured by UV absorbance at 254 nm. The HPLC consists of an XTerra RP18 column (3.5 μm, 3.9 mm × 100 mm) from the manufacturer Waters (Milford, MA, USA) and two LC-10AD pumps, a SPD-M10A VP PDA detector, and a SIL-HT autosampler, all from the manufacturer Shimadzu (Kyoto, Japan). For preparative tasks a XTerra RP18 column (7 μm, 19 mm × 150 mm) from the manufacturer Waters (Milford, MA, USA) and two LC-20AD pumps were used. The mobile phase was in all cases a gradient of methanol/ water (starting at 95% water going to 5% water).
Mass spectrometry analyses were performed with a Finnigan MAT710C (Thermo Separation Products, San Jose, CA, USA) for the ESIMS spectra and with a LTQ (linear ion trap) Orbitrap XL hybrid mass spectrometer (Thermo Fisher Scientific, Bremen, Germany) for the HRMS-ESI (high resolution mass spectrometry) spectra. For the HRMS analyses the signal for the isotopes with the highest prevalence was given and calculated ( 35 Cl, 79 Br).