Mercury vx 300 nmr spectrometer

Melting points were measured on an Electrothermal IA 9000 series digital melting point apparatus (Bibby Sci. Lim. Stone, Staffordshire, UK). IR spectra were measured on PyeUnicamSP 3300 and Shimadzu FTIR 8101 PC infrared spectrophotometers (Shimadzu, Tokyo, Japan) in potassium bromide discs. NMR spectra were measured on a Varian Mercury VX-300 NMR spectrometer (Varian, Inc., Karlsruhe, Germany) operating at 300 MHz (¹HNMR) and run in deuterated dimethylsulfoxide (DMSO-d₆). Chemical shifts were related to that of the solvent. Mass spectra were recorded on a Shimadzu GCMS-QP1000 EX mass spectrometer (Tokyo, Japan) at 70 eV. Elemental analyses were measured by using a German made Elementarvario LIII CHNS analyzer. 2-(4-Methyl-2-phenylthiazole-5-carbonyl)-N-phenylhydrazinecarbothioamide (3) [31 (link)], and hydrazonoyl halides 4a–c [32 ] were prepared as reported in the respective literature.

The FT-IR 460 PLUS Spectrophotometer was used to capture IR spectra in Potassium bromide plates in the 4000–400 cm⁻¹ range. DMSO-d6 was used as a solvent to acquire the proton nuclear magnetic resonance spectra using a Varian Mercury VX-300 NMR Spectrometer. Shimadzu UV-3101PC was used for measuring the electronic absorption spectra where ethanol was used as solvent. Shimadzu TGA-50H was used for carrying out the thermal analysis. TG-DTG measurements were performed in an environment of N₂ at temperatures ranging from 0 °C to 1000 °C where the sample mass was precisely measured out in an aluminum crucible. Elemental analysis was carried out using a PerkinElmer 2400 CHN elemental analyzer. With a Gouy balance, a Sherwood scientific magnetic scale, and H_g[Co(CSN)⁴] as the signing, the magnetic susceptibilities of the powdered materials were tested at ambient temperature. CONSORT K410 was used to analyze the molar conductance of 1 × 10⁻³ M solutions of the ligands and their complexes in ethanol. Each experiment was run at room temperature with freshly made solutions. The progress of the reaction was monitored by thin-layer chromatography (TLC).

All melting points were determined on an electro thermal Gallen Kamp melting point apparatus (lain George, Calgary, Canda) and are uncorrected. IR (cm⁻¹) spectra were recorded on KBr disk on a FTIR-8201 spectrophotometer (Shimadzu, Tokyo, Japan). ¹H NMR and ¹³C NMR spectra were measured in deuterated dimethyl sulfoxide (DMSO-d6) using a Mercury VX-300 NMR spectrometer (Varian, Inc., Palo Alto, California 94304 USA). Mass spectra were recorded on a Shimadzu GCMS-QP1000 EX mass spectrometer (Tokyo, Japan) at 70 eV. Measurements of the elemental analysis were carried out at the Microanalytical Centre of Cairo University, Giza, Egypt. All reactions were followed by TLC (Silica gel, Merck, Kenilworth, NJ, USA). Hydrazonoyl halides were prepared as previously reported [32 (link), 33 (link)].

The structure of extracted PHB was analyzed using FTIR and GC-MS, and the produced spectrum was compared with the PHB standard (Sigma cat no: 29435-48-1). NICOLET 380 FTIR (Thermo Scientific, China) was applied to identify the functional groups in the produced polymer [33 (link)]. To determine the chemical composition of the produced polymer, GC-TSQ mass spectrometer (Thermo Scientific, USA) was used [34 (link)]. NMR analysis of the extracted PHB was performed according to the method described by Kanzariya et al. [35 (link)]. ¹H NMR spectra were recorded on a Varian Mercury VX-300 NMR spectrometer. H1 spectra were run at 300 MHz in deuterated dimethylsulphoxide (DMSO-d6).

All reagents used in synthesis of compounds were commercially available of at least 97% purity. Solvents were commercially available materials of reagent grade. Melting points (mp) were uncorrected and were determined using a Buchi SMP-20 apparatus (Buchi Labortechnik, Flawil, Switzerland). The ¹HNMR (300 MHz) were obtained in CDCl₃ with a Varian Mercury-VX 300 NMR spectrometer (Varian Inc., Palo Alto, CA, USA) using TMS as an internal standard. Spectral data includes chemical shifts in ppm, multiplicities, constant couplings in Hz, number of protons, protons’ positions. Multiplicities are abbreviated as follow: s (singlet), d (doublet), dd (doublet of doublets), ddd (double doublet of doublets), ddt (double doublet of triplets), t (triplet), quint (quintet), and m (multiplet). The LC/MS system consisted of an Acquity UPLC system (Waters Corporation, Milford, MA, USA) coupled to a Waters TQD mass spectrometer (electrospray ionization mode ESI-tandem quadrupole). All the LC/MS analyses were carried out using an Acquity UPLC BEH C18, 1.7 µm, 2.1 × 100 mm² column. A flow rate of 0.3 mL/min and a gradient of (5–95)% B over 10 min and then 100% B over 2 min was used. Eluent A: water/0.1% HCOOH; eluent B: acetonitrile/0.1% HCOOH. LC/MS data were obtained by scanning the first quadrupole in 0.5 s in a mass range from 50 to 1000 Da; 8 scans were added to produce the final spectrum.

Melting points were measured with an IA 9000-series digital melting-point apparatus (Bibby Sci. Lim. Stone, Staffordshire, UK). IR spectra were recorded in potassium bromide discs on FTIR 8101 PC infrared spectrophotometers (Shimadzu, Tokyo, Japan). NMR spectra were recorded on a Mercury VX-300 NMR spectrometer (Varian, Inc., Karlsruhe, Germany) operating at 300 MHz (¹H-NMR) and run in deuterated dimethylsulfoxide (DMSO-d₆). Chemical shifts were related to that of the solvent. Mass spectra were recorded on a Shimadzu GCeMS-QP1000 EX mass spectrometer (Tokyo, Japan) at 70 eV. Elemental analyses were measured using an ElementarVario LIII CHNS analyzer (elementar Analysensysteme GmbH, Hanau, Germany). Ultrasonication was carried out in an ElmaRD-7700 apparatus (Singen, Germany). The electric supply was 230 V, A.C. 50 Hz, 1 phase; the ultrasonic frequency was 36 KHz and the ultrasonic power 100 W. 1,4-Dioxo-3,4-dihydrophthalazine-2(1H)-carbothioamide (1) [36 (link)] and hydrazonoyl halides 2 and 5 [37 (link)] were prepared as previously reported in the respective literature.