302 a spectrophotometer

Chromatographic solvents were purchased from Fisher Scientific, UK, and used without further purification. Optical rotations were measured in methanol on a JASCO DIP-360 digital polarimeter using a 10 cm cell. Ultraviolet spectra were recorded on a Hitachi UV 3200 spectrophotometer in MeOH. Infrared spectra were recorded on a JASCO 302-A spectrophotometer. ESIMS was recorded on a Finnigan LCQ with a Rheos 4000 quaternary pump (Flux Instrument). EIMS were recorded on a Varian MAT 311A spectrometer (70 eV). EIMS was performed on a JEOL HX 110 mass spectrometer. The ¹H and ¹³C NMR spectra were recorded at 600 and 150 MHz, respectively, on a Bruker AMX 600 NMR spectrometer. Chemical shifts are reported in δ (ppm). Column chromatography was carried out on silica gel (70–230 mesh, Merck) and flash silica gel (230–400 mesh, Merck). TLC was performed on Merck precoated silica gel 60 F₂₅₄ aluminum foil, using ceric sulfate spray reagent for visualization. The purity of compounds was investigated by HPLC. The degree of purity of the positive control compound was ≥98%, while that of the isolated compounds was ≥95%. All reagents used were analytical grade.

The spectra of UV were reported on spectrophotometric instrument Hitachi UV-3200. IR spectral data were measured using a JASCO 302-A spectrophotometer. EI–MS (m/z) were recorded on JEOL JMS-HX-110 mass spectrometer. At 400 MHz, the spectra of ¹H-NMR were observed on the instrument named Bruker AM-400 AMX spectrometers with the respective frequency data system. TMS of compounds was used as a reference (mainly internally). The spectra of ¹³C-NMR (broadband and DEPT or GASPE) were accomplished on the same instruments at 75 MHz, 100 MHz, and 125 MHz, respectively. The values of the chemical shift were expressed as ppm (δ) and the coupling constants (J) values were expressed in Hz.