Example 4
Materials and Methods
Chemicals were purchased from Aldrich Chemical Company (Gillingham, Dorset), Alfa Aesar (Heysham, Morecambe, Lancashire) and Carbosynth Limited (Compton, Berkshire), unless otherwise noted, and were used without further purification. Solvents were purchased as anhydrous. Petrol was the fraction boiling between 40-60° C. TLC was carried out using aluminium plates pre-coated with silica gel (Kieselgel 60 F254, 0.2 mm, Merck, Darmstadt, Germany). Visualization was by UV light. 1H NMR spectra were recorded on either a Bruker 300 MHz or 400 MHz spectrometer using the residual proton(s) in the deuterated solvents as internal standards. HPLC analyses were performed on a Shimadzu Prominence instrument with diode array detection. LCMS analyses were performed on a Shimadzu 2010EV instrument operating in positive or negative electrospray (ESI) mode. Automated chromatography was performed on a Biotage Isolera purification system.