Unity plus 400 mhz

Most the chemicals were purchased from SigmaeAldrich (St. Louis, MO, USA), Merck (Berlin, Germany) or Alfa-Aesar (Ward Hill, MA, USA). Reactions in ultrasound bath were performed in a Unique EM-804 TGR instrument, with a frequency of 40 kHz and a nominal power of 180 W, and without external heating. Precoated aluminum sheets (silica gel 60 F254, Merck) were used for thinlayer chromatography (TLC) and spots were visualized under UV light. Elemental analysis was performed with a Carlo Erba instrument model E-1110. IR spectra in KBr pellets were acquired at Bruker FT-IR spectrophotometer. 1 H and 13 C NMR were recorded on a Uni-tyPlus 400 MHz and Bruker AMX-300 MHz spectrometer, using DMSO-d 6 as a solvent and trimethylsilane (TMS) as the internal standard. Splitting patterns were defined as; s, singlet; d, doublet; dd, double doublet; t, triplet; q, quartet; m, multiplet. Chemical shift values were given in ppm. DEPT was employed to confirm the carbon assignment.

1 H NMR measurements were performed on an Advance (Bruker, Rheinstetten, Germany) Unity Plus 400 MHz nuclear magnetic resonance spectrometer using D 2 O as the solvent. FT-IR spectra were obtained between 400 and 4500 cm -1 on a Nicolet NEXUS-670 (Nicolet Instrument Corporation, WI, USA) at room temperature. The spectra. The number-average molecular weight (Mn), weight-average molecular weight (Mw), and polydispersity (Mw/Mn) of the polymers were determined by gel permeation chromatography (GPC) at 35 o C using a Waters 1525 chromatograph equipped with a Waters 2414 refractive index detector. Tetrahydrofuran (THF) was used as the mobile phase at a flow rate of 1 mL/min. The GPC columns were standardized with narrow dispersity polystyrene in molecular weights ranging from 4.7×10 6 to 2350.

All reagents were used as purchased from commercial sources (Sigma-Aldrich, Acros Organics, Vetec or Fluka). Progress of the reactions was followed by thin-layer chromatography (silica gel 60 F 254 in aluminum foil). Chemical identity was confirmed by NMR and IR spectroscopy and accurate mass. IR was determined in KBr pellets. For NMR, we used a Varian Unity Plus 400 MHz (400 MHz for 1 H and 100 MHz for 13 C) and Bruker AMX-300 MHz (300 MHz for 1 H and 75.5 MHz for 13 C) instruments. DMSO-d 6 and CDCl 3 -d 6 were purchased from CIL or Sigma-Aldrich. Chemical shifts are reported by ppm and multiplicities are given as: s (singlet), d (doublet), t (triplet),q (quartet), m (multiplet) integration, and coupling constants (J) in hertz. Structural assignments corroborated by DEPT experiments. Mass spectrometry experiments were performed on a Q-TOF spectrometer (nanoUPLC-Xevo G2 Tof, Waters) or LC-IT-TOF (Shimadzu). When otherwise specified, ESI was carried out in the positive ion mode. Typical conditions were: capillary voltage of 3 kV and cone voltage of 30 V, and peak scan between 50 and 1000 m/z.