All chemicals and regents used for this study were analytical grade and used without further purification. 1,10-phenanthroline monohydrate (BDH chemical Ltd., Poole, England), copper (II) acetate monohydrate [Cu(CO2CH3)2·H2O], triethylamine, NaHCO3, NaOH, and Mueller-Hinton agar were purchased from Loba Chemie PVT Ltd., Addis Ababa. Metformin hydrogen chloride (Met.HCl) and ciprofloxacin hydrogen chloride (Cip.HCl) were obtained from Cadila Pharmaceuticals PLC, Ethiopia. Methanol, ethanol, HCl, DMSO, ethyl acetate and dichloromethane (DCM) were purchased from Alpha Chemika, Addis Ababa, Ethiopia. Thin Layer Chromatography (MERCK Silica gel 60 F254) together with UV Cabinet (UV-Vis lamp at 254 and 365 nm) were used to monitor the progress of the chemical reactions. The melting points of the complexes were determined using capillary tubes (Thiele tube). UV-Vis spectrophotometer (SM-1600 Spectrophotometer), FTIR (Perkin-Elmer BX spectrometer, Shimadzu Corporation, Japan), TGA/DTC (DTG-60H SHIMADZU thermal analyzer) and High resolution mass spectra (Waters-LCT-Premier mass spectrometer) were used to characterize the synthesized metal complexes.
Merck silica gel 60 f254
Manufactured by Merck Group
Sourced in Germany
Merck silica gel 60 F254 is a type of thin-layer chromatography (TLC) material. It is composed of silica gel particles with a fluorescent indicator, F254, which allows for the visualization of separated compounds under ultraviolet (UV) light.
Automatically generated - may contain errors
Lab products found in correlation
Merck silica gel 60, by Merck Group (9 mentions)
Silica gel 60, by Merck Group (4 mentions)
Avance 300, by Bruker (2 mentions)
Sodium hydroxide (naoh), by Loba Chemie (1 mentions)
Waters lct premier mass spectrometer, by Waters Corporation (1 mentions)
Triethylamine, by Loba Chemie (1 mentions)
Methanol, by Alpha Chemika (1 mentions)
Ethanol, by Alpha Chemika (1 mentions)
Ethyl acetate, by Alpha Chemika (1 mentions)
Mueller hinton agar (mha), by Loba Chemie (1 mentions)
Dimethyl sulfoxide (dmso), by Alpha Chemika (1 mentions)
1100 series lc msd spectrometer, by Agilent Technologies (1 mentions)
Avance spectrometer, by Bruker (1 mentions)
Cholesterol chol, by Avanti Polar Lipids (1 mentions)
Glacial acetic acid, by Merck Group (1 mentions)
Multiskan go microplate spectrophotometer, by MultiSciences Biotech (1 mentions)
Nicolet is10 spectrophotometer, by Bruker (1 mentions)
Am 300, by Bruker (1 mentions)
Zorbax eclipse xdb c18, by Agilent Technologies (1 mentions)
Rp c18, by Merck Group (1 mentions)
46 protocols using merck silica gel 60 f254
1
Synthesis and Characterization of Metal Complexes
2
Spectroscopic Characterization of Organic Compounds
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All reactants and reagents were purchased from Alfa Aesar and Sigma–Aldrich as “synthesis grade.” Chemical reactions were monitored by analytical thin-layer chromatography (TLC) using several solvent systems with different polarity on Merck Silica Gel 60 F254 (0.040–0.063 mm) with detection by UV. Merck Silica Gel 60 (0.040–0.063 mm) was used for column chromatography. 1H NMR and 13C NMR spectra were recorded on a Varian 300 MHz (USA) spectrometer using the residual signal of the deuterated solvent as internal standard. Splitting patterns of signals are indicated as singlet (s), doublet (d), triplet (t), multiplet (m), broad (br), and doublet of doublet (dd). The values of chemical shifts (δ) are reported in ppm and coupling constants (J) in hertz (Hz). Electrospray ionization-mass spectrometric (ESI-MS) were acquired with an Agilent 1100 series LC/MSD spectrometer equipped with a multimode ion source and by using methanol as solvent.
3
Comprehensive Compound Characterization Protocol
4
Synthesis of Substituted Benzaldehyde Derivatives
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Ethyl bromopyruvate (technical grade, 90%), thiourea (ACS reagent) benzaldehyde (ReagentPlus® 99%), salicylaldehyde (reagent grade, 98%), 3-hydroxybenzaldehyde (AR ≥ 99%), 4-hydroxybenzaldehyde (Analytical standard), 4-hydroxy-3-methoxybenzaldehyde (ReagentPlus® 99%), acetophenone (Analytical standard), 2′-hydroxyacetophenone (ReagentPlus® 99%),. Ethanol (absolute, ACS reagent) and glacial acetic acid (100%, anhydrous for analysis ACS, ISO reagent) were used purchased from Sigma Aldrich and Merck. Synthesized compounds were purified by recrystallization in appropriate solvents and examined through thin layer chromatography (Merck Silica gel 60 F254). Melting points were determined by using digital Gallenkamp model MPD BM 3.5 apparatus. Characterization of synthesized compounds was made through spectrophotometric analysis; FT-IR (Thermoscientific NICOLET IS10 spectrophotometer), 1H & 13C NMR (Bruker AM-300 and AM-100 spectrophotometer) using DMSO and CDCl3 respectively. Elemental analysis values were recorded on Model ANALYST 2000 CHNS, Perkin Elmer Analyzer. Multiskan™ GO Microplate Spectrophotometer was used to quantify synthesized compounds for accuracy, precision and sensitivity [26 ].
5
Enantioselective Biocatalytic Reductions
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Kits of TAs and KREDs were purchased from Codexis. The cultures for overexpression of the IREDs were inoculated from E. coli BL21 (DE3) glycerol stocks from Greifswald University containing the respective IREDs in a pET 22b(+) vector. The standard procedure for expression was followed as described in ref. 11a. TA variants from ArRmut11 were overexpressed in E. coli and used as lyophilized cells (for more details about these TAs, see ref. 16). For the enzymatic reactions, commercially available solvents were used. Thin‐layer chromatography was performed on precoated TLC plates of Merck silica gel 60F254, using potassium permanganate as developing reagent. For column chromatography, Merck silica gel 60 (particle size, 40–63 μm) was used. 1H NMR and proton‐decoupled 13C NMR spectra were obtained using a 300 MHz spectrometer using the δ scale (ppm) for chemical shifts; calibration was made on the CDCl3 (13C; 76.95 ppm) or the residual CHCl3 (1H; 7.26 ppm) signals. HPLC analyses to determine degree of conversions were carried out in an Agilent RR1200 HPLC system, using a reversed phase column (Zorbax Eclipse XDB−C18, RR, 18 μm, 4.6×50 mm, Agilent). HPLC analyses to determine ee were performed on a Hewlett Packard 1100 LC liquid chromatograph, using normal phase columns (Chiralcel OJ−H and Chiralpak IA).
6
Spectroscopic Analysis of Organic Compounds
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UV spectra were recorded using a Thermo spectrometer. IR spectra were recorded using a JASCO FT/IR-4100 spectrometer (JASCO, Easton, MD, USA). The 1D- and 2D-NMR spectra were obtained using Varian Unity Inova 400 MHz and 500 MHz spectrometers with tetramethylsilane (TMS) as an internal standard, and the chemical shifts were recorded as δ values (ppm). Mass spectra were recorded using a Thermo Scientific™ (Q Exactive) EASY-nLC 1000 spectrometer (San Jose, CA, USA). Silica gel (Merck, Darmstadt, Germany; 63–200 µm particle size), RP-C18 (Merck; 75 µm particle size), sephadex LH-20 (Pharmacia, Uppsala, Sweden ), and dianion HP-20 (Supelco, St. Louis, MI, USA) were used for column chromatography. TLC was performed using Merck Silica gel 60 F254 and RP-C18 F254 plates (Merck, Darmstadt, Germany). Preparative high-performance liquid chromatography (HPLC) was performed using a Water System with a UV detector 2996 (Waters, Miford, MA, USA) and a YMC-Triart C18 column (10 mm × 250 mm, 5 μm particle size; YMC Co., Ltd., Kyoto, Japan). Compounds were visualized after spraying with aqueous 10% H2SO4 and heating for 3–5 min.
7
Analytical and Purification Techniques
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All commercial reagents and chromatography solvents were used as obtained unless otherwise stated. Ethanol, toluene, ethyl acetate, hexanes, anhydrous sodium sulfate (Na2SO4, BDH), Pd(PPh3)4 (Strem Chemicals). Anhydrous solvents were distilled over appropriate drying agents prior to use. Analytical thin layer chromatography (TLC) was performed on Merck Silica gel 60 F254. Merck Silica gel 60 (0.063–0.2 mm) was used for column chromatography. Visualization of TLC was accomplished with UV light (254 nm). NMR spectra were recorded on a Bruker-Avance 400 MHz spectrometer. The residual solvent protons (1H) or the solvent carbon (13C) were used as internal standards. 1H-NMR data are presented as follows: chemical shift in ppm (δ) downfield from trimethylsilane (multiplicity, integration, coupling constant). The following abbreviations are used in reporting NMR data: s, singlet; bs, broad singlet; d, doublet; t, triplet; q, quartet; dq, doublet of quartets; dd, doublet of doublets; m, multiplet. High resolution mass spectra were recorded using Chemical Ionization (CI) and electrospray ionization (ESI) techniques.
8
Compound Structure Analysis by NMR
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The structures of compounds were unambiguously assessed by 1H NMR and 13C NMR recorded on a Bruker AC 400 or 100 (Milan, Italy), respectively, spectrometer and analyzed using the TopSpin software package (version 2.1). Chemical shifts were measured using the central peak of the solvent. Column chromatography purifications were performed under “flash” conditions using Merck 230–400 mesh silica gel. TLC was carried out on Merck silica gel 60 F254 plates, which were visualized by exposure to an aqueous solution of ceric ammonium molibdate.
9
Synthesis and Characterization of Organic Compounds
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All chemicals and reagents were obtained from Aldrich (Sigma-Aldrich, Bangalore, India) and Alfa-Aesar (Johnson Matthey Company, India). Reactions were monitored by TLC, performed on Merck silica gel 60 F-254, and visualization on TLC was achieved by UV light or iodine indicator. Column chromatography was performed with Merck 60–120 mesh silica gel. Melting points were taken on a hot-plate microscope apparatus. IR spectra were obtained with a Bruker Tensor 27 spectrometer (KBr disk). NMR spectra were recorded with a Varian 500 spectrometer with CDCl3 as solvent and TMS as internal standard (500 and 125 MHz for 1H NMR and 13C NMR spectra, respectively). High-resolution mass (ESI) was obtained with a Bruker Micro-TOF spectrometer.
10
Synthesis and Spectroscopic Analysis of Organic Compounds
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All of the chemicals utilized during
the reactions were obtained from Spectrochem, India. 1H
NMR and 13C NMR spectra were recorded at room temperature
on Varian 400 MHz and 100 MHz spectrometers, respectively. Chemical
shift values were
displayed with reference to TMS as an internal standard. DMSO-d6 was used as the solvent to prepare the samples.
Chemical shifts were expressed in δ (ppm) and coupling constants
(J) in Hertz. The splitting pattern abbreviations
are as follows: s, singlet; d, doublet; t, triplet; q, quartet; m,
unresolved multiplet; dd, doublet of the doublet. Column chromatography
was performed with Merck silica gel 60 (230–400 mesh). Analytical
thin-layer chromatography was carried out using Merck silica gel 60F254, and iodine was used as a developing reagent. IR spectra
were recorded on an FTIR IR Affinity-1 Shimadzu spectrophotometer.
The CHNS analysis was recorded on Elementar Vario El-III.
the reactions were obtained from Spectrochem, India. 1H
NMR and 13C NMR spectra were recorded at room temperature
on Varian 400 MHz and 100 MHz spectrometers, respectively. Chemical
shift values were
displayed with reference to TMS as an internal standard. DMSO-d6 was used as the solvent to prepare the samples.
Chemical shifts were expressed in δ (ppm) and coupling constants
(J) in Hertz. The splitting pattern abbreviations
are as follows: s, singlet; d, doublet; t, triplet; q, quartet; m,
unresolved multiplet; dd, doublet of the doublet. Column chromatography
was performed with Merck silica gel 60 (230–400 mesh). Analytical
thin-layer chromatography was carried out using Merck silica gel 60F254, and iodine was used as a developing reagent. IR spectra
were recorded on an FTIR IR Affinity-1 Shimadzu spectrophotometer.
The CHNS analysis was recorded on Elementar Vario El-III.
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