General Methods. Nuclear Magnetic Resonance (NMR) spectra were recorded on a 400 MHz spectrometer. 1 H and 13 C spectra were referenced relative to the solvent residual peaks and chemical shifts (δ) reported in ppm downfield of trimethylsilane (CDCl 3 δ H: 7.26 ppm, δ C: 77.0 ppm; CD 3 OD δ H: 3.31 ppm, δ C: 49.05 ppm; DMSO-d6 δ H: 2.50 ppm, δ C: 39.52 ppm). Coupling constants (J) are reported in Hertz and rounded to 0.5 Hz. Splitting patterns are abbreviated as follows: singlet (s), doublet (d), triplet (t), quartet (q), multiplet (m), broad (br) or some combination of these. Low resolution mass spectra were recorded by staff at the Northumbria University Newcastle and King's College London. Positive and negative electrospray ionisation spectrometry (ESI-MS) were conducted using a Thermo LCQ Advantage mass spectrometer by direct injection. GC-MS analyses were performed on a Thermo Electron Co. Focus GC coupled to a Thermo DSQ1 mass spectrometer and an AI3000 Auto Injector. Aliquots of the compound dissolved in DCM (5 μL) were injected onto a DB-5MS (30 m × 0.25 mm i.d. × 0.15 μm film thickness) column at 250 °C. The oven temperature was set at 40 °C for 4 min and raised at 15 °C/min to 135 °C, then at 5 °C/min to 250 °C and holded at 250°C for 5 minutes. The carrier gas flow was 1.0 mL/min. The mass spectrometer was operated in the full scan mode. The transfer line and ion source temperatures were 250 °C and 200 °C, respectively. Thin layer chromatography (TLC) was performed using commercially available pre-coated plates (Macherey-Nagel alugram. Sil G/UV254) and visualized with UV light at 254 nm; K 2 MnO 4 or Ninhydrin dips were used to reveal the products. Flash column chromatography was carried out using Fluorochem Davisil 40-63u 60Å. Petrol refers to the fraction of light petroleum ether boiling between 40 and 65 °C. All other solvents and commercially available reagents were used as received. All chemicals and solvents were used as supplied, unless noted otherwise.
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