Agilent 660 ftir spectrometer

Materials and instrumentation 3,4,5-Trimethoxytoluene (97%) and 2,3-dimethoxy-5-methyl-1,4-benzoquinone (99%) were obtained from Aldrich, 2,3dimethoxytoluene (98%) and 2,4,6-trimethoxytoluene (97%) were purchased from Alfa, 3,5-dimethoxytoluene (99%), 1,2,3trimethoxybenzene (98%) and 1,3,5-trimethoxybenzene (99%) were obtained from Acros. Acetonitrile (Panreac, HPLC grade) was dried and stored over activated 4 Å molecular sieves. All the other compounds were the best available reagent grade and used without further purification. The concentration of H 2 O 2 (ca. 35 wt% aqueous solution) was determined iodometrically prior to use. GC analyses were performed using a gas chromatograph Chromos GC-1000 equipped with a flame ionization detector and a quartz capillary column BPX5 (30 m × 0.25 mm). GC-MS analyses were carried out using an Agilent 7000B system with a triple-quadrupole mass-selective detector Agilent 7000 (HP-5 ms quartz capillary column 30 m × 0.25 mm). 1 H, 31 P and 51 V NMR spectra were recorded on a Brüker AVANCE-400 spectrometer at 400.130, 161.67 and 105.24 MHz, respectively. Chemical shifts for P and V, δ, were determined relative to 85% H 3 PO 4 and VOCl 3 , respectively. Infrared spectra were recorded with KBr pellets on an Agilent 660 FTIR spectrometer.