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All reactions that required anhydrous or airless conditions were carried by standard procedures under an argon atmosphere. Commercially available reagents from Tansoole and Adamas-beta were used as received. The solvents were dried by distillation over the appropriate drying reagents. 1 H NMR spectra were recorded on commercial instruments (400 MHz and 600 MHz). Chemical shifts were reported in ppm from tetramethylsilane with the solvent resonance as the internal standard (CDCl3, δ = 7.28). Spectra were reported as follows: chemical shift (δ ppm), multiplicity (s = singlet, d = doublet, t = triplet, q = quartet, m = multiplet), coupling constants (Hz), integration and assignment. 13 C NMR spectra were collected on commercial instruments (101 MHz and 151 MHz) with complete proton decoupling. Chemical shifts were reported in ppm from the tetramethylsilane with the solvent resonance as internal standard (CDCl3, δ = 77.0). Mass spectra were recorded on a ThermoQuest Finnigan LCQDECA system equipped with an ESI source. The single crystal X-ray diffraction measurement was performed on a Xcalibur, Eos diffractometer. The crystal was kept at 293.15 K during data collection. Using Olex2 1 ,

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Publisher

American Chemical Society (ACS)

Language

EN

Category

nonfiction