The melting point values were recorded on a Thermocouple digital melting point apparatus (Mettler Toledo LLC, Columbus, OH, USA) and are uncorrected. The IR spectra, on the other hand, were recorded as powders using a Bruker VERTEX 70 FT-IR Spectrometer (Bruker Optics, Billerica, MA, USA) with a diamond ATR (attenuated total reflectance) accessory by using the thin-film method. For column chromatography, we employed Merck kieselgel 60 (0.063–0.200 mm) as stationary phase (Merck KGaA, Frankfurt, Germany). NMR spectra were obtained as DMSO-d6 solutions on a Varian Mercury 300 MHz NMR spectrometer (Varian Inc., Palo Alto, CA, USA) or Agilent 500 MHz NMR spectrometer (Agilent Technologies, Oxford, UK) and the chemical shifts are quoted relative to TMS peak. Low- and high-resolution mass spectra were recorded at an ionization potential of 70 eV using Micromass Autospec-TOF (double focusing high resolution) instrument (Waters Corp., Milford, MA, USA).
Thermocouple digital melting point apparatus
Manufactured by Mettler Toledo
Sourced in United States
The Thermocouple digital melting point apparatus is a laboratory equipment used to determine the melting point of solid substances. It employs a thermocouple to precisely measure and display the temperature of the sample.
Automatically generated - may contain errors
Lab products found in correlation
Vertex 70 ftir spectrometer, by Bruker (5 mentions)
Agilent 500 mhz nmr spectrometer, by Agilent Technologies (4 mentions)
Merck kieselgel 60 0.063 0 200 mm, by Merck Group (4 mentions)
Mercury 300 mhz nmr spectrometer, by Agilent Technologies (2 mentions)
Micromass autospec tof double focusing high resolution instrument, by Waters Corporation (2 mentions)
Waters synapt g2 quadrupole time of flight mass spectrometer, by Waters Corporation (2 mentions)
Micromass autospec tof, by Waters Corporation (1 mentions)
5 protocols using thermocouple digital melting point apparatus
1
Analytical Techniques for Chemical Characterization
2
Characterization of 2,4-Dihydroxy-5-iodoacetophenone
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The melting point (mp.) values of the prepared compounds were recorded on a Thermocouple digital melting point apparatus (Mettler Toledo LLC, Columbus, OH, USA) and are uncorrected. Their infrared (IR) spectra were recorded using the thin-film method on a Bruker VERTEX 70 FT-IR Spectrometer (Bruker Optics, Billerica, MA, USA) equipped with a diamond attenuated total reflectance (ATR) accessory. The Merck kieselgel 60 (0.063–0.200 mm) (Merck KGaA, Frankfurt, Germany) was used as a stationary phase for column chromatography. The proton (1H-) and carbon-13 (13C-) nuclear magnetic resonance (NMR) spectra of the prepared compounds were obtained as CDCl3 or dimethyl sulfoxide-d6 (DMSO-d6) solutions using Agilent 500 MHz NMR spectrometer (Agilent Technologies, Oxford, UK). The chemical shifts are quoted relative to the tetramethylsilane (TMS) peak as an internal reference standard. The high-resolution mass spectra were recorded at the University of Stellenbosch using a Waters Synapt G2 Quadrupole Time-of-flight mass spectrometer (Waters Corp., Milford, MA, USA) at an ionization potential of 70 eV. The synthesis and analytical data for 2,4-dihydroxy-5-iodoacetophenone, were reported in our previous investigation [23 (link)].
3
Synthesis and Characterization of Compounds
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The melting points of the compounds prepared in this investigation were recorded on a Thermocouple digital melting point apparatus (Mettler Toledo LLC, Columbus, OH, USA). Their IR spectra were recorded as powders using a Bruker VERTEX 70 FT-IR Spectrometer (Bruker Optics, Billerica, MA, USA) equipped with a diamond attenuated total reflectance (ATR) accessory. For column chromatography, we used the Merck kieselgel 60 (0.063–0.200 mm) (Merck KGaA, Frankfurt, Germany) as stationary phase. The NMR spectra were obtained as DMSO-d6 solutions using Varian Mercury 300 MHz NMR spectrometer (Varian Inc., Palo Alto, CA, USA) and the chemical shifts are quoted relative to the residual proton signal in the deuterated solvent. The mass spectra were recorded at an ionization potential of 70 eV using Waters Synapt G2 Quadrupole Time-of-flight mass spectrometer (Waters Corp., Milford, MA, USA) at the University of Stellenbosch. The synthesis and analytical data of compounds 1a –d , which are known have been described before [18 (link)].
4
Characterization of 2-amino-5-iodobenzamide
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The melting point values of the test compounds were recorded on a Thermocouple digital melting point apparatus (Mettler Toledo LLC, Columbus, OH, USA). The infrared (IR) spectra were recorded using the thin-film method on a Bruker VERTEX 70 FT-IR Spectrometer (Bruker Optics, Billerica, MA, USA) equipped with an ATR (diamond attenuated total reflectance) accessory. Merck kieselgel 60 (0.063–0.200 mm) (Merck KGaA, Frankfurt, Germany) was used as a stationary phase for column chromatography. The 1H-NMR and 13C-NMR spectra of the prepared compounds were obtained as deuterated dimethyl sulfoxide ((CD3)2SO) solutions using Agilent 500 MHz NMR spectrometer (Agilent Technologies, Oxford, UK) operating at 500 MHz and 125 MHz for 1H and 13C, respectively. The chemical shifts are quoted relative to tetramethylsilane (TMS) used as an internal reference standard (δ = 0.00 ppm) or a residual protonated solvent. The high-resolution mass spectra were recorded at an ionization potential of 70 eV using Micromass Autospec-TOF (double focusing high resolution) instrument (Waters Corp., Milford, MA, USA). The synthesis and analytical data for 2-amino-5-iodobenzamide (1 ) have been reported in our previous study [25 (link)]. Recombinant human AChE (BioLegend) and BChE (Cloud-Clone Corp.) were purchased via Biocom Africa (Pty) Ltd. (Centurion, Pretoria, South Africa).
5
Spectroscopic Characterization of Compounds
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The melting point values of the test compounds were recorded on a Thermocouple digital melting point apparatus (Mettler Toledo LLC, Columbus, OH, USA). The infrared (IR) spectra were recorded using the thin-film method on a Bruker VERTEX 70 FT-IR Spectrometer (Bruker Optics, Billerica, MA, USA) equipped with an ATR (diamond attenuated total reflectance) accessory. Merck kieselgel 60 (0.063–0.200 mm) (Merck KGaA, Frankfurt, Germany) was used as a stationary phase for column chromatography. The 1H NMR and 13C NMR spectra were recorded as deuterated chloroform (CDCl3) or dimethyl sulfoxide ((CD3)2SO) solutions using Agilent 500 MHz NMR spectrometer (Agilent Technologies, Oxford, UK) operating at 500 MHz and 125 MHz for 1H and 13C, respectively. The chemical shifts are quoted relative to tetramethylsilane (TMS) used as an internal reference standard (δ = 0.00 ppm) or to residual protonated solvent. Data are presented as follows: chemical shift (ppm), multiplicity (s = singlet, d = doublet, t = triplet, q = quartet, sept = septet, m = multiplet, br = broad), coupling constant J (Hz), and integration. The high-resolution mass spectra were recorded at an ionization potential of 70 eV using Micromass Autospec-TOF (double focusing high resolution) instrument (Waters Corp., Milford, MA, USA).
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