1.0 General Synthetic Methods for Synthesis of 2 in Main Paper

Abstract:

All reactions were carried out under an atmosphere of dry nitrogen using standard Schlenk techniques. Dichloromethane was purified and dried using an Innovative Technology SPS-400 before use, triethylamine was distilled over calcium sulfate, other solvents were standard reagent grade and used as received. No special precautions were taken to exclude air or moisture during workup except where otherwise indicated. The catalyst PdCl2 (PPh3) 2 was synthesized by literature methods. 1 All other reagents were commercially available and used as received. NMR spectra were recorded at 23 ºC on a Varian NMR Systems 700 (1H, 699.7 MHz; 11B, 224.5 MHz; 13C, 175.9 MHz; 29Si, 139.0 MHz) or a Varian NMR Systems 600 spectrometer (19F, 564.3 MHz) using CDCl3 or CD3CN/D2O (2: 1 (v/v)) as the solvent. Chemical shifts were determined relative to internal CHCl3 (1H δ= 7.26 ppm, CDCl3), internal CDCl3 (13C δ= 77.16 ppm, CDCl3), internal CHD2CN (1H δ= 1.94 ppm, CD3CN/D2O (2: 1 (v/v))), internal CD3CN (13C δ= 1.32 ppm, CD3CN/D2O (2: 1 (v/v))) 2 external BF3· Et2O (11B δ= 0.0), external CF3C6H5 (19F δ=–63.72 ppm) and external tetramethylsilane (29Si δ= 0.0 ppm). Assignment of the 1H and 13C NMR data was supported by gradient selected 13C, 1H HMQC and HMBC experiments. EI-MS spectra were recorded on a Thermo-Finnigan Corporation Trace GC-MS and ESI-MS were recorded on a Waters Ltd TQD mass spectrometer in positive mode. Elemental analyses were performed at the London Metropolitan University.

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