As 400 mercury plus nmr spectrometer

Chemistry Materials and Methods Melting points were determined using a Stuart SMP30 (Staffordshire, ST15 OSA, U.K.) melting point apparatus and are not corrected. IR spectra of the compounds were recorded as potassium bromide pellets on a PerkinElmer 100 Fourier transform (FT)-IR spectrophotometer (PerkinElmer, Inc., MA, U.S.A.). 1 (link) H-and 13 C-NMR spectra were recorded with a Varian AS 400 Mercury Plus NMR spectrometer (Varian, Palo Alto, CA, U.S.A.) operated at 400 and 100 MHz for 1 H and 13 (link) C, respectively, in deutero-dimethyl sulfoxide (DMSO). Chemical shifts are given in ppm (δ) with tetramethylsilane (TMS) as an internal standard. Abbreviations for data quoted are: s (singlet), d (doublet), t (triplet), quin (quintet), m (multiplet), br s (broad singlet). HR-MS of the title compounds were recorded on a HPLC-TOF Waters Micromass LCT Premier XE (Milford, MA, U.S.A.) mass spectrometer using an electrospray ion source (ESI). All chemicals, reagents and solvents used for synthesis were high-grade commercial products and they were purchased from Sigma, Acros, Fluka, U.S.A., and Merck Companies. Reactions were checked by TLC on pre-coated silica gel aluminum plates (Kieselgel 60, F 254 , E. Merck, Germany); spots were visualized by UV at 254 nm.