Silica gel 60n

Manufactured by Kanto Chemical

Sourced in Japan

Silica gel 60N is a type of silica gel used as a stationary phase in column chromatography. It is a porous, amorphous form of silicon dioxide with a high surface area. Silica gel 60N is chemically inert and has a neutral pH, making it suitable for a wide range of chromatographic separations. The 'N' in the name indicates that the silica gel has a normal particle size distribution.

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Lab products found in correlation

Silica gel 60 f254, by Merck Group (5 mentions) Jms dx303hf, by JEOL (4 mentions) Tlc silica gel 60 f254, by Merck Group (4 mentions) Avance 600, by Bruker (4 mentions) Jnm eca600, by JEOL (3 mentions) Tlc sheets silica 60 f254, by Merck Group (3 mentions) Cosmosil 5c18 ar 2, by Nacalai Tesque (3 mentions) Eca 500, by JEOL (3 mentions) Eca 500 spectrometer, by JEOL (3 mentions) Ecs 400, by JEOL (3 mentions) Silica gel 60 f254 plate, by Merck Group (3 mentions) Rp 18 f254, by Merck Group (3 mentions) Jnm ecx400, by JEOL (2 mentions) Jms t100lp mass spectrometer, by JEOL (2 mentions) Tlc silica gel 60 f254 aluminum sheet, by Merck Group (2 mentions) Avance 600 spectrometer, by Bruker (2 mentions) Silica gel 70 f254 tlc plates, by Fujifilm (2 mentions) Jms t100lc, by JEOL (2 mentions) Unity plus 400 mhz spectrometer, by Bruker (2 mentions) Microtof focus 2 mass spectrometer, by Bruker (2 mentions)

Close spelling variants of this product

Chemical silica gel 60N Spherical silica gel 60N Silica gel

72 protocols using silica gel 60n

Spectroscopic and Computational Analysis

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¹H NMR (400 MHz and 600 MHz) and ¹³C NMR (151 MHz) spectra were recorded with a JEOL JNM-ECX 400, a JEOL JNM-ECP 400 and a JEOL JNM-ECA 600 spectrometers by using tetramethylsilane as an internal standard. The HR-MALDI-TOF mass spectra were measured by a Bruker Autoflex II spectrometer using positive ion mode.
UV/Vis absorption spectra were measured with a JASCO UV/Vis/NIR spectrophotometer V-570.
TLC and gravity column chromatography were performed on Art. 5554 (Merck KGaA) plates and silica gel 60N (Kanto Chemical), respectively. All other solvents and chemicals were reagent-grade quality, obtained commercially, and used without further purification. For spectral measurements, spectral-grade solvents were purchased from Nacalai Tesque.
All DFT calculations were performed with a Gaussian 09 program package. The geometries were fully optimized at the Becke's three-parameter hybrid functional combined with the Lee–Yang–Parr correlation functional abbreviated as the B3LYP level of density functional theory. The 6-31G(d) bases set implemented was used for structure optimizations and frequency analyses.

Mei P., Matsumoto A., Hayashi H., Suzuki M., Aratani N, & Yamada H. (2018). 1,3-Phenylene-bridged naphthalene wheels synthesized by one-pot Suzuki–Miyaura coupling and the complex of the hexamer with C60. RSC Advances, 8(37), 20872-20876.

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Synthesis and Characterization of Organic Compounds

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Melting points were determined using Yanaco melting point device and were uncorrected. Infrared (IR) spectra were recorded by Jasco FT/IR-6600 spectrophotometer as KBr disks and were expressed in wavenumber (cm⁻¹). NMR spectra were measured using Bruker Advance III HD at 400 MHz for ¹H NMR, 100 MHz for ¹³C NMR and 376 MHz for ¹⁹F NMR in deuterated CDCl₃, DMSO-d₆ or MeOH-d4 using tetramethyl silane (TMS) as an internal standard. Coupling constant values (J) were determined in Hertz (Hz) and chemical shifts (δ) were expressed in ppm. High resolution mass spectra (HRMS) were measured with Thermo Fisher Scientific LTQ Orbitrap XL spectrophotometer using electrospray ionization (ESI) and were expressed as [M+H]⁺ or [M+Na]⁺ at Natural Science Research and Development Center, Hiroshima University, Japan. The reaction mixtures were monitored by thin layer chromatography (TLC) using Merck silica gel 60F₂₅₄ aluminum sheets. Column chromatography was conducted using silica gel 60 N, 63–210 μm that was purchased from Kanto Chemical Co. Inc. Unless otherwise mentioned, all solvents and chemical reagents were commercially available and were used without further purification.

Elbadawi M.M., Eldehna W.M., Wang W., Agama K.K., Pommier Y, & Abe M. (2021). Discovery of 4-alkoxy-2-aryl-6,7-dimethoxyquinolines as a new class of topoisomerase I inhibitors endowed with potent in vitro anticancer activity. European journal of medicinal chemistry, 215, 113261.

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Purification and Characterization of Triphenylene Derivatives

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Triphenylene and hexaacetoxytriphenylene were purchased from Tokyo Chemical Industry (TCI). They were used after reprecipitation from dichloromethane and hexane for the spectroscopic and electrochemical measurements. All solvents and reagents of the best grade available were purchased from commercial suppliers and were used without further purification. Column flash chromatography was performed on silica gel (Kanto Chemical Silica gel 60N, 40–50 μm or 100–210 μm). We used an LC-9204 apparatus equipped with a pump (JAI PI-60, flow rate 2.5 mL min^–1), a UV detector (JAI UV-3740) and two columns (JAIGEL 2H and 1H, 40 × 600 mm for each). All experiments except single crystal X-ray diffraction measurements were performed at room temperature. ¹H NMR and ¹³C NMR spectra were recorded on a 400 MHz spectrometer JEOL JNM-A400, JNM-Al400, or JNM-ECX 400, using the solvent peak as the reference standard, with chemical shifts given in parts per million. CDCl₃ was used as a solvent for NMR measurements. MALDI-TOF mass spectra were recorded on a Bruker Ultraflex.

Aoki T., Sakai H., Ohkubo K., Sakanoue T., Takenobu T., Fukuzumi S, & Hasobe T. (2014). Ultrafast photoinduced electron transfer in face-to-face charge-transfer π-complexes of planar porphyrins and hexaazatriphenylene derivatives †Electronic supplementary information (ESI) available: 1H, 13C NMR and MALDI-TOF mass spectra, cyclic voltammograms, fluorescence spectra, fluorescence titration spectra, 1H NMR titration, femtosecond laser-induced transient absorption spectral measurement data, and DFT data. See DOI: 10.1039/c4sc02787f Click here for additional data file.. Chemical Science, 6(2), 1498-1509.

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Synthesis of Compound (I-14) from (I-18) and Methyl Isobutyl Ketone

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Example 7

[Figure (not displayed)]

1.35 Parts of a compound represented by formula (I-18) and 3 parts of methyl isobutyl ketone were mixed, followed by stirring at 23° C. for 30 minutes. To the mixed solution thus obtained, 2.40 parts of an aqueous 2.5% p-toluenesulfonic acid solution was added dropwise, followed by stirring at 23° C. for 1 hour. To the reaction mixture thus obtained, 10 parts of methyl isobutyl ketone and 5 parts of ion-exchanged water were added, and after stirring at 23° C. for 30 minutes, the organic layer was isolated through separation. To the organic layer thus obtained, 5 parts of ion-exchanged water was added, and after stirring at 23° C. for 30 minutes, the organic layer was isolated through separation. This water washing operation was repeated five times. The organic layer thus obtained was concentrated, and then the concentrated mixture was isolated from a column (silica gel 60 N (spherical, neutral) 100-210 μm; manufactured by Kanto Chemical Co., Inc., developing solvent: n-heptane/ethyl acetate=1/1) to obtain 0.22 part of a compound represented by formula (I-14).

MASS (Mass Spectrometry): 333.0 [M+H]⁺

US11822244B2. Compound, resin, resist composition and method for producing resist pattern (2023-11-21). SUMITOMO CHEMICAL COMPANY, LIMITED [JP]. Inventors: Tatsuro Masuyama [JP], Takuya Nakagawa [JP], Koji Ichikawa [JP].

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Comprehensive NMR and Mass Spectrometry Analysis

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One- and two-dimensional ¹H NMR spectra were recorded on a JNM-ECZ500R spectrometer at 500 MHz, and ¹³C NMR spectra were recorded on the same instrument at 125 MHz (JEOL, Tokyo, Japan). HRESIMS spectra were measured on a JMS-T100LP mass spectrometer (JEOL, Tokyo, Japan). HPLC separations were performed with a Jasco Chromatography Data Station ChromNAV system using reverse-phase HPLC columns (ODS-P, InertSustain, Tokyo, Japan). Silica gel plates (Merck F254), ODS gel plates (Merck F254) and silica gel 60 N (Kanto Chemical, Tokyo, Japan) were used for analytical TLC and flash column chromatography. All solvents used throughout the experiments were obtained from Kanto Chemical Co. (Tokyo, Japan).

Kotajima M., Choi J.H., Kondo M., D’Alessandro-Gabazza C.N., Toda M., Yasuma T., Gabazza E.C., Miwa Y., Shoda C., Lee D., Nakai A., Kurihara T., Wu J., Hirai H, & Kawagishi H. (2022). Axl, Immune Checkpoint Molecules and HIF Inhibitors from the Culture Broth of Lepista luscina. Molecules, 27(24), 8925.

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Silica Gel Column Chromatography

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Column chromatography
separations were performed using silica gel 60 N (spherical, neutral,
particle size 63–210 μm; Kanto Chemical). All commercially
available reagents and solvents were of reagent grade and were used
without purification. The solvents for measurements were all spectral
grade and were used without purification.

Yamauchi M., Fujiwara Y, & Masuo S. (2020). Slow Anion-Exchange Reaction of Cesium Lead Halide Perovskite Nanocrystals in Supramolecular Gel Networks. ACS Omega, 5(24), 14370-14375.

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Chemical Synthesis and Characterization

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The chemicals were purchased from Sigma-Aldrich (St. Louis, MO, USA), Honeywell Fluka (Morristown, NJ, USA), Kanto Chemical (Tokyo, Japan), Nacalai Tesque (Kyoto, Japan), Tokyo Chemical Industry (Tokyo, Japan), and FUJIFILM Wako (Osaka, Japan). The commercially available reagent-grade chemicals were used without further purification. The reaction progress was monitored by thin-layer chromatography (TLC) on TLC silica gel 60 F₂₅₄ aluminum sheets (Merck, Darmstadt, Germany). The flash column chromatography was performed on Silica Gel 60N (40–100 mesh, Kanto Chemical, Tokyo, Japan). Melting points (mp) were determined on a Yanaco melting point apparatus (Kyoto, Japan) and were uncorrected. ¹H and ¹³C NMR spectra were recorded on a Bruker Avance 600 spectrometer (600 MHz) (Billerica, MA, USA). Mass spectrometry (MS) and high-resolution mass spectrometry (HRMS) data were recorded on a JEOL (Tokyo, Japan) JMS-DX303HF using positive fast atom bombardment (FAB) technique with 3-nitrobenzyl alcohol as the matrix.

Ciftci H.I., Radwan M.O., Sever B., Hamdy A.K., Emirdağ S., Ulusoy N.G., Sozer E., Can M., Yayli N., Araki N., Tateishi H., Otsuka M., Fujita M, & Altintop M.D. (2021). EGFR-Targeted Pentacyclic Triterpene Analogues for Glioma Therapy. International Journal of Molecular Sciences, 22(20), 10945.

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Spectroscopic Characterization of Natural Products

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¹H NMR spectra (one- and two-dimensional) were recorded on a Jeol lambda-500 spectrometer or a JNM-ECZ500R spectrometer at 500 MHz, and ¹³C NMR spectra were recorded on the same instrument at 125 MHz (JEOL, Tokyo, Japan). HRESIMS spectra were measured on a JMS-T100LP mass spectrometer (JEOL, Tokyo, Japan). The specific rotation values were measured with a Jasco DIP-1000 polarimeter (Jasco, Tokyo, Japan). HPLC separations were performed with a Jasco Chromatography Data Station ChromNAV system using reverse-phase HPLC columns (CAPCELL PAK C18 AQ, Osaka soda, Osaka, Japan; COSMOSIL PBr, nacalai tesque, Kyoto, Japan; InerSustain Amide, InertSustain Phenyl, GL Science, Tokyo, Japan). Silica gel plate (Merck F254), ODS gel plate (Merck F254) and silica gel 60 N (Kanto Chemical, Tokyo, Japan) were used for analytical TLC and for flash column chromatography. All solvents used throughout the experiments were obtained from Kanto Chemical Co. (Tokyo, Japan).

Wu J., Ohura T., Ogura R., Wang J., Choi J.H., Kobori H., D’Alessandro-Gabazza C.N., Toda M., Yasuma T., Gabazza E.C., Takikawa Y., Hirai H, & Kawagishi H. (2023). Bioactive Compounds from the Mushroom-Forming Fungus Chlorophyllum molybdites. Antibiotics, 12(3), 596.

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Analytical and Spectroscopic Characterization

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The starting materials, reagents, and solvents were purchased and used without further purification. We used Silica gel 70 F254 TLC plates (Wako) for analytical Thin-layer chromatography (TLC), while Silica gel 60 N (spherical, neutral, Kanto Chemical) were for column chromatography. For preparative flash chromatography, used were an automated system (Smart Flash EPCLC AI-580S, Yamazen Corp., Japan) equipped with universal columns of silica gel. Melting points and IR spectra were determined with a MP-500P (Yanaco) and a Nicolet 6700 spectrometer with anATR attachment, respectively. ¹H and ¹³C NMR spectra were determined on a JEOL ECA-500 instrument (500 MHz for ¹H and 126 MHz for ¹³C). Mass spectra were obtained with a high-resolution electro-spray ionization mass spectrometer, JMS-T100LC (JEOL). UV/visible absorption spectra were determined with a spectrophotometer, Cary 60 (Agilent Technologies) (scan speed 600 nm/min; data interval 1 nm). BL and chemiluminescence spectra were measured with a precision spectrophotometer, AB-1850 (ATTO) (data interval: 1 nm). BL intensities were monitored using luminometers, AB-2270 (ATTO) and GL-201A (Microtec Co.). BL imaging was performed with a multifunctional in vivo imaging system (IVIS Spectrum, PerkinElmer).

Tamaki S., Kitada N., Kiyama M., Fujii R., Hirano T., Kim S.B, & Maki S. (2021). Color-tunable bioluminescence imaging portfolio for cell imaging. Scientific Reports, 11, 2219.

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Synthesis and Characterization of Novel Compounds

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Compounds Lin1 and Fus4 were commercially available, whereas Compounds Lin2, Lin3, and Fus2 were produced by synthesis (reaction schemes and individual details of the synthetic procedure are indicated in Methods S1). Reagents and solvents were obtained from commercial suppliers and used without further purification, unless otherwise stated. Reactions were carried out under a positive atmosphere of nitrogen, unless otherwise stated. Reactions were monitored by thin layer chromatography (TLC) carried out on Merck TLC Silica gel 60 F₂₅₄, using shortwave UV light as the visualizing agent and phosphomolybdic acid in EtOH and heat as developing agent. Flash column chromatography was performed using Kanto Chemical Silica gel 60 N (spherical, 40–50 μm). ¹H NMR spectra were recorded on Varian Unity Plus 400 MHz spectrometer or Bruker Avance III HD 500 MHz spectrometer and were calibrated using residual undeuterated solvent as the internal references (CDCl₃: 7.26 ppm; MeOH-d₄: 3.31 ppm, acetone-d₆: 2.05 ppm; DMSO-d₆: 2.50 ppm). The following abbreviations were used to explain NMR peak multiplicities: s = singlet, d = doublet, t = triplet, q = quartet, p = pentet, m = multiplet, br = broad. Low-resolution and high-resolution mass spectra were recorded on Bruker micrOTOF focus II mass spectrometer using electrospray ionization time-of-flight (ESI-TOF) reflectron experiments.

Rujas E., Insausti S., Leaman D.P., Carravilla P., González-Resines S., Monceaux V., Sánchez-Eugenia R., García-Porras M., Iloro I., Zhang L., Elortza F., Julien J.P., Saéz-Cirión A., Zwick M.B., Eggeling C., Ojida A., Domene C., Caaveiro J.M, & Nieva J.L. (2020). Affinity for the Interface Underpins Potency of Antibodies Operating In Membrane Environments. Cell reports, 32(7), 108037.

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