Thin-layer chromatography (TLC) sep arations of F5, F10’, and F2” were performed using commercially available plates (silica gel 60 F254-precoated TLC plates; Merck, Germany) and suitable solvent systems at room temperature. For the detection of the main compounds, different spray reagents (Dragendorff, potassium hydroxide, vanillin-sulphuric acid, and Liebermann- Burchard reagents) were used. The detection of the characteristic components was also performed via observing the developed chromatograms under long-wave and short-wave UV light (366 and 254 nm, respectively) (26 ).
Precoated tlc plates silica gel 60 f254
Manufactured by Merck Group
Sourced in Germany
Precoated TLC plates (silica gel 60 F254) are a type of thin-layer chromatography (TLC) plates used for analytical and preparative purposes. The plates are coated with a layer of silica gel 60 F254, which is a common adsorbent material used in TLC. The F254 indicates that the silica gel is fluorescent, allowing for the visualization of separated compounds under UV light.
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Lab products found in correlation
Silica gel 60, by Merck Group (1 mentions)
Tlc scanner 3, by CAMAG (1 mentions)
Horizontal developing chamber, by CAMAG (1 mentions)
Twin through glass tank, by CAMAG (1 mentions)
Linomat 5, by CAMAG (1 mentions)
Methanol, by Fujifilm (1 mentions)
Dichloromethane, by Fujifilm (1 mentions)
Ethyl acetate, by Fujifilm (1 mentions)
Tetrahydrofuran thf, by Fujifilm (1 mentions)
Silica gel 60, by Nacalai Tesque (1 mentions)
Linoleic acid, by Merck Group (1 mentions)
1 ethyl 3 3 dimethylaminopropyl carbodiimide hydrochloride, by Merck Group (1 mentions)
Cinnamic acid, by Merck Group (1 mentions)
2 2 diphenyl 1 picrylhydrazyl radical dpph, by Merck Group (1 mentions)
10 undecenoic acid, by Merck Group (1 mentions)
Tert butylhydroquinone tbhq, by Merck Group (1 mentions)
P coumaric acid, by Merck Group (1 mentions)
Sinapic acid, by Merck Group (1 mentions)
Caffeic acid, by Merck Group (1 mentions)
Ferulic acid, by Merck Group (1 mentions)
7 protocols using precoated tlc plates silica gel 60 f254
1
TLC Separation and Detection of Compounds
2
Melting Point Determination and Compound Characterization
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Thermonic melting point apparatus was used in order to determine the melting points of compounds and are not corrected. Thin layer chromatography (TLC) checked the purity of compounds by using silica gel 60 F 254 pre-coated TLC plates (E. Merck). Chromatographic separations were carried out on silica gel 60 (0.063–0.200 or 0.040–0.063 mm, E. Merck). Elemental analyses (C, H, N) were done on CarloErba-1108 elemental analyzer, and obtained results were found within the ±0.4% of theoretical values. Perkin Elmer-881 and Paragon 500 FTIR infrared spectrophotometer were employed for the determination of functional group in compounds, and v was marked in cm-1. Bruker DRX-300 FT NMR spectrometer was used to get the 1H NMR spectra at 300 MHz by employing CDCl3/DMSO-d6 solvent. Chemical shifts are given in δ (ppm) using tetramethylsilane as internal standard. Peak multiplicities are expressed as follows: s, singlet; d, doublet; t, triplet; m, multiplet. Jeol-JMS D-300 instrument was involved in recording the mass spectra. Reaction sequences leading to synthesis of present series is outlined in Scheme 1 .
3
Thin Layer Chromatography for Compound Analysis
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After trying number of TLC in different solvent system, maximum number of spot was confirmed by TLC in a specific solvent system; thereafter that solvent system was used for analysis. Prepared samples were filtered and 8 µL of each of the solutions were separately applied on Silica gel 60 F254 precoated TLC plates, 5x10 cm (Merck, Germany) with the help of CamagLinomat-V (CAMAG, Switzerland) applicator and the plate was eluted to a distance of 8.5 cm at room temperature (25°C) in specific developed solvent system. The sample solution was applied to 6-mm wide band using CamagLinomat-V automated TLC applicator with the nitrogen flow providing a delivery speed of 150 nL/s from the syringe. Plates were developed in a Camag twin through glass tank pre-saturated with the mobile phase for 40 min. The plate was developed horizontally in Camag horizontal developing chamber (10 × 10 cm) at the room temperature. The scanning was carried out at 254 nm and 366 nm with a Camag TLC scanner III using the Wincats1.2.3 software.
4
Synthesis and Purification of Organometallic Precursor
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Dichloromethane, N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), ethyl acetate, hexane, methanol, tetrahydrofuran (THF), lithium bromide (LiBr), and chloro(1,5-cyclooctadiene)(η5-pentamethylcyclopentadienyl)ruthenium(II) (Cp*RuCl(COD)) were purchased from FUJIFILM Wako Pure Chemical Corp. (Osaka, Japan). A solution of tetrabutylammonium fluoride (TBAF) in THF (1 M) was purchased from Tokyo Chemical Industry Co., Ltd. (Tokyo, Japan). Copper(I) bromide (CuBr), sodium chloride (NaCl), sodium sulfate (Na2SO4), and tetrasodium ethylenediaminetetraacetate (EDTA·4Na) were purchased from Nacalai Tesque, Inc. (Kyoto, Japan). Pentamethylcyclopentadienylbis(triphenylphosphine)ruthenium(II) chloride (Cp*RuCl(PPh3)2) was purchased from Sigma–Aldrich (St. Louis, MO, USA). Merck precoated TLC plates (Silica gel 60 F254) were used for thin layer chromatography (TLC) analysis in this work. Silica gel 60 (Nacalai Tesque, spherical, neutrality) was used for column chromatography to purify the products. THF and DMF were dried with flame-dried molecular sieves 4A. Other reagents were used without further purification. tBuAH and t-butyl 6-(t-butyldimethylsilyl)-4-hydroxy-5-hexynoate (1 ) were prepared according to the procedure reported previously [26 (link)].
5
Synthesis and Radical Scavenging Evaluation
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10-Undecenoic acid, 1,1’-azobis(cyclohexanecarbonitrile) (ABCN), hydroxybenzotriazole (HOBt) and 1-ethyl-3-(3’-dimethylaminopropyl)carbodiimide hydrochloride (EDC·HCl), cysteamine hydrochloride, cinnamic acid, sinapic acid, ferulic acid, p-coumaric acid, caffeic acid, α-tocopherol (α-TP), tert-butylhydroquinone (TBHQ), linoleic acid (LA) and 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical were purchased from Sigma–Aldrich (St.Louis, USA), and pre-coated TLC plates (silica gel 60 F254) were purchased from Merck (Darmstadt, Germany). All solvents were purchased from Sd Fine Chemicals (Mumbai, India) and were of the highest grade of purity available.
6
Synthesis of Barium Carbonate Compounds
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An aqueous solution of formaldehyde (36 wt%), barium carbonate (BaCO3) and N,N,N′,N′-tetraethylethylenediamine were purchased from Sigma-Aldrich (St. Louis, MO). Calcium hydroxide (Ca(OH)2), silver(i ) oxide (Ag2O), alumina (Al2O3), imidazole, pyridine and acetylacetone were purchased from FUJIFILM Wako Pure Chemical Corp. (Osaka, Japan). Barium hydroxide octahydrate (Ba(OH)2·8H2O), sodium hydroxide (NaOH), potassium hydroxide (KOH), triethylamine, 2-picoline, 3-picoline, acetic acid and ammonium acetate were purchased from Nacalai Tesque, Inc. (Kyoto, Japan). Lithium oxide monohydrate (LiOH·H2O), 2-(dimethylamino)ethanol and acetonitrile for HPLC were purchased from Kishida Chemical Co., Ltd. (Osaka, Japan). Magnesium hydroxide (Mg(OH)2), 1,4-diazabicyclo[2.2.2]octane (DABCO) and N-methylpiperidine were purchased from Kanto Chemical Co. Inc. (Tokyo, Japan). Amberlite® IR-120 H and IRA-910 Cl were purchased from Sigma-Aldrich (St. Louis, MO). Amberlite® IRA-910 Cl was used after exchanging Cl− ions to OH− ions (Amberlite® IRA-910 OH) by washing with 1.0 M NaOH. For thin layer chromatography (TLC), Merck precoated TLC plates (silica gel 60 F254) were used. Water was purified with a Millipore Milli-Q system. Other reagents were used without further purification.
7
Synthesis and Evaluation of Ferulic Acid Derivatives
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Ferulic acid and 2, 2-diphenyl-1-picrylhydrazyl (DPPH) radical were purchased from Fluka (Buchs, Switzerland) . tert-Butyl dimethyl silyl chloride, dimethyl amino pyridine (DMAP) were purchased from ACROS (New Jersey, USA) .
Butyric anhydride, butanol were purchased from Aldrich (USA) . Camphor sulfonic acid (CSA) was purchased from Lancaster (England) . Silica gel (60-120 mesh) for column chromatography was purchased from Acme Synthetic Chemicals (Mumbai, India) and pre-coated TLC plates (silica gel 60 F 254 ) were purchased from Merck (Darmstadt, Germany) . All solvents were purchased from SD-fine chem. (Mumbai, India) and were of the highest grade of purity, and were used without further purification. The bacterial test organisms and the fungal strains were obtained from the Institute of Microbial Technology, Chandigarh, India. The medium was procured from Himedia Laboratories (Mumbai, India) .
Butyric anhydride, butanol were purchased from Aldrich (USA) . Camphor sulfonic acid (CSA) was purchased from Lancaster (England) . Silica gel (60-120 mesh) for column chromatography was purchased from Acme Synthetic Chemicals (Mumbai, India) and pre-coated TLC plates (silica gel 60 F 254 ) were purchased from Merck (Darmstadt, Germany) . All solvents were purchased from SD-fine chem. (Mumbai, India) and were of the highest grade of purity, and were used without further purification. The bacterial test organisms and the fungal strains were obtained from the Institute of Microbial Technology, Chandigarh, India. The medium was procured from Himedia Laboratories (Mumbai, India) .
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