Anhydrous solvents
were dried and stored
over molecular sieves (3 Å), and all other reagents and solvents
were used as received. Anhydrous iron(III) chloride was purchased
from Sigma Aldrich and stored in a glovebox under nitrogen. Reactions
performed under an inert atmosphere were carried out using Schlenk
glassware using nitrogen as the inert gas. Flash column chromatography
was performed using silica gel (230–400 mesh). NMR experiments
were performed on either a Brüker Avance 400 MHz instrument
and JEOL 600 MHz ECZ600R instrument at 298 K. Chemical shifts are
quoted in ppm relative to tetramethylsilane, using the solvent residual
peak of CDCl3 (δH 7.26, δC 77.00) as a reference
standard. TGA was performed with a PerkinElmer TGA 8000 and by heating
the polymer (0.5–3 mg) from 30 to 600/800 °C in atmospheric
pressure, with a T-ramp of 5 °C min–1 under
oxygen flux (30 mL min–1). IR spectra were obtained
with a Perkin Elmer spectrum two FT-IR spectrometer (diamond crystal)
in the 4000–400 cm–1 interval at room temperature.
were dried and stored
over molecular sieves (3 Å), and all other reagents and solvents
were used as received. Anhydrous iron(III) chloride was purchased
from Sigma Aldrich and stored in a glovebox under nitrogen. Reactions
performed under an inert atmosphere were carried out using Schlenk
glassware using nitrogen as the inert gas. Flash column chromatography
was performed using silica gel (230–400 mesh). NMR experiments
were performed on either a Brüker Avance 400 MHz instrument
and JEOL 600 MHz ECZ600R instrument at 298 K. Chemical shifts are
quoted in ppm relative to tetramethylsilane, using the solvent residual
peak of CDCl3 (δH 7.26, δC 77.00) as a reference
standard. TGA was performed with a PerkinElmer TGA 8000 and by heating
the polymer (0.5–3 mg) from 30 to 600/800 °C in atmospheric
pressure, with a T-ramp of 5 °C min–1 under
oxygen flux (30 mL min–1). IR spectra were obtained
with a Perkin Elmer spectrum two FT-IR spectrometer (diamond crystal)
in the 4000–400 cm–1 interval at room temperature.