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Reactions were performed in oven or flame dried glassware, either under positive argon pressure, or in sealed tubes flushed with argon. Microwave irradiations were performed using BIOTAGE Smith Initiator in sealed reaction vessels. The temperature on the outer surface of the vial was measured via infrared thermometer. The microwave output power is regulated by the software algorithm, so that the preselected maximum temperature is maintained for the desired reaction time. Unless otherwise noted, reagents and anhydrous solvents were purchased from commercial sources (Sigma Aldrich, TCI, Strem Chemicals etc.) and were used without any further purification. n-BuLi was titrated according to the method of J. Suffert. 1 Reactions were monitored by thin-layer chromatography (TLC) on Merck aluminium sheets silica gel 60 F254, which were visualized with UV light or KMnO4 stain. The crude products were purified by flash column chromatography on Merck silica gel (particle size 40-63 μm). Nuclear magnetic resonance (NMR) spectra were recorded in CDCl3 Bruker Avance III 400MHz or 500MHz BBFO+ probe spectrometer. Proton chemical shifts are reported in ppm (δ), relatively to residual CHCl3 (δ 7.26

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Publisher

American Chemical Society (ACS)

Language

EN

Category

nonfiction