Kiesel gel 60 f254

All reagents and solvents were of general
purpose or analytical grade and were purchased from Sigma-Aldrich
Ltd., Fisher Scientific, Fluorochem, or Acros. ¹H and ¹³C NMR data were recorded on a Bruker AVANCE DPX500 spectrometer
operating at 202, 500, and 125 MHz. Chemical shifts (δ) are
quoted in ppm, and J values are quoted in Hz. In
reporting spectral data, the following abbreviations were used: s
(singlet), d (doublet), t (triplet), q (quartet), dd (doublet of doublets),
td (triplet of doublets), and m (multiplet). All of the reactions
were carried out under a nitrogen atmosphere and were monitored using
analytical thin-layer chromatography on precoated silica plates (Kieselgel
60 F254, BDH). Compounds were visualized by illumination under UV
light (254 nm) or by the use of KMnO₄ stain followed by
heating. Flash column chromatography was performed with silica gel
60 (230–400 mesh) (Merck). High-performance liquid chromatography
(HPLC) was carried out on a SHIMADZU Prominence-i quaternary low-pressure
gradient pump with a Prominence-i UV detector (190 to 700 nm). All
solvents for HPLC were of HPLC grade and purchased from Fisher Scientific.
HPLC data analysis was performed using the SHIMADZU Lab Solutions
software package. The purity of the final compounds was determined
by HPLC, and they were all of ≥95% purity unless stated otherwise.

Chemicals and solvents employed in chemical synthesis were of analytical grade and, when necessary, were purified and dried by standard methods. Reactions were monitored by thin-layer chromatography (TLC) using pre-coated silica gel plates (Kieselgel 60 F254, BDH), and spots were visualized under UV light (254 nm). Melting points were determined using a Gallenkamp melting point apparatus and are uncorrected. Column chromatography was performed with Merck silica gel 60 (40–60 μM). Both 1H NMR and 13C NMR spectra were recorded on a Bruker Avance 500 MHz spectrometer. Chemical shifts were expressed in parts per million (ppm) relative to tetramethylsilane. Coupling constant (J) values were represented in hertz (Hz), and the signals were designated as follows: s, singlet; d, doublet; t, triplet; m, multiplet. Mass spectroscopic data were obtained through electrospray ionization (ESI) mass spectrum (Bruker MicroTOF instrument). Elemental analysis (% CHN) was run by combustion analysis through an outsourced service (Medac Ltd., Surrey, UK).

All solvents, reagents and chemicals were bought from Sigma Aldrich. The used solvents were purified according to the standard methods. TLC was carried out on the plates of silica gel (Merck Kiesel gel 60F254, BDH) to monitor the progress of all synthesized compounds homogeneity and reactions. Microwave reactions were carried out with microwave reactor Anton Paar (monowave 300) using 10 mL borosilicate glass vials. All melting points were measured on a digital Stuart electric melting point apparatus “SMP3” and were uncorrected. Infrared spectra measurements (cm⁻¹) were determined using KBr disks on a PerkinElmer 293 spectrophotometer. The ¹H-NMR and ¹³C-NMR spectra were measured on a Varian Mercury 300 MHz spectrometer. All synthesized compounds were dissolved in DMSO–d₆ as a solvent using tetramethyl silane as an internal standard. A GC-2010 Shimadzu Gas chromatography mass spectrometer (EI, 70 eV) was used for Mass spectrometry measurements. A Perkin-Elmer CHN-2400 analyzer was used for elemental microanalyses (CHN), the data were found to be in good agreement within ± 0.4% of the theoretical values. No-carrier-added [¹³¹I]NaI was received as a gift from RPF (Radioisotopes-Production-Facility), Egyptian Atomic Energy Authority (EAEA). A NaI (Tl) scintillation counter (Scaler Ratemeter SR7 model, the United Kingdom) was used for γ-ray radioactivity measurement.

All solvents, reagents and chemicals were bought from Sigma Aldrich. TLC (Merck Kiesel gel 60F254, BDH) to monitor the progress of all synthesized compounds. Microwave reactions were carried out with microwave reactor Anton Paar (monowave 300). All melting points were measured on a digital Stuart electric melting point apparatus “SMP3”. Infrared spectra measurements were determined using KBr disks on PerkinElmer 293 spectrophotometer. The ¹H-NMR and ¹³C-NMR spectra were measured on a Varian Mercury 75 MHz spectrometer. A GC-2010 Shimadzu Gas chromatography mass spectrometer (EI, 70 eV) was used for Mass spectrometry measurements. A Perkin-Elmer CHN-2400 analyzer was used for elemental microanalyses (CHN). No-carrier-added [¹³¹I] NaI was received as a gift from RPF (Radioisotopes-Production-Facility), Egyptian Atomic Energy Authority (EAEA). A NaI (Tl) scintillation counter (Scaler Ratemeter SR7 model, the United Kingdom) was used for γ-ray radioactivity measurement.