Siliaflash p60

Manufactured by Silicycle

Sourced in Canada

SiliaFlash® P60 is a high-performance flash chromatography silica gel designed for the purification of organic compounds. It features a particle size of 40-63 μm and a pore size of 60 Å, providing efficient separation and purification.

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Lab products found in correlation

Sephadex lh 20, by GE Healthcare (1 mentions) Total antioxidant capacity assay kit, by Beyotime (1 mentions) Poroshell 120 ec c18 2.7 μm, by Agilent Technologies (1 mentions) Unity inova spectrometer, by Agilent Technologies (1 mentions) Avance 3 500, by Bruker (1 mentions) Avance 3 400, by Bruker (1 mentions) Toluene, by Merck Group (1 mentions) Octylamine, by Tokyo Chemical Industry (1 mentions) Milli q system, by Merck Group (1 mentions) Tlc silica gel 60 f254, by Merck Group (1 mentions)

16 protocols using siliaflash p60

Optimized Synthesis of Bishydroxylated Pulegone

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Example 1

Both the selectivity and yields obtained for the α,α′-bishydroxylation of pulegone can depend on the quality of KHMDS and control of the temperature. Separation of the diastereomeric products was improved via use of wet silica gel, prepared as follows: Silica gel (SiliaFlash® P60, particle size 40-63 microns [230 to 400 mesh], purchased from Silicycle, 950 g) was slowly mixed with deionized water (50 mL) in a 1-liter media bottle. The silica was then vigorously shaken for five minutes, and then allowed to equilibrate for 12 h before use as normal for silica gel purification. The product obtained by this method was typically 97% pure by ¹H NMR analysis, containing some minor oxaziridine-derived products.

US09862696B2. Synthetic route to anhydroryanodol, ryanodol and structural analogues (2018-01-09). CALIFORNIA INSTITUTE OF TECHNOLOGY [US]. Inventors: Sarah Reisman [US], Kangway V. Chuang [US], Chen Xu [US].

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Purification and Characterization of Organic Compounds

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Reagents and solvents were
bought from commercially accessible vendors such as Sigma-Aldrich,
AK Scientific, and Fisher Scientific and used without further purification.
Thin layer chromatography (TLC) was used to monitor the reactions’
progress on 0.25 mm silica gel 60 F254 plates from Merck and visualized
by staining in ninhydrin solution. Normal and reverse-phase column
chromatography was performed to purify the compounds using SiliaFlash
P60 (40–63 μm) 60 Å silica gel and SiliaBond C18
(40–63 μm) 60 Å silica gel from SiliCycle, respectively.
The yields of the compounds were determined after purification. The
chemical structures of all intermediates and final products were characterized
by nuclear magnetic resonance (¹H NMR and ¹³C NMR) on a Bruker AMX-300 MHz NMR and 500 MHz spectrometer. ¹³C NMR spectra were fully decoupled. Chemical shifts were
reported in parts per million (ppm) using deuterated solvents chloroform-d (7.26 ppm), MeOD (3.31 ppm), and HOD (4.79 ppm) as internal
standards. Matrix-assisted laser desorption ionization mass spectrometry
(MALDI-MS) spectra were recorded on Bruker Daltonics ultraflex MALDI-time-of-flight
(TOF)/TOF and MS-electrospray ionization mass spectrometers. Purity
of the final compounds was determined by high-performance liquid chromatography
(HPLC) from Thermo Scientific HPLC using a reversed-phase Synergi
100 Å C18 (50 × 2 mm) column from Phenomenex.

Dhiman S., Ramirez D., Arora R., Gandhi K., Wimalasekara R., Arthur G., Kumar A, & Schweizer F. (2023). Trimeric Tobramycin/Nebramine Synergizes β-Lactam Antibiotics against Pseudomonas aeruginosa. ACS Omega, 8(32), 29359-29373.

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Purification and Characterization of Organic Compounds

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All chemicals were purchased from the Uni-Onward Corporation in Taiwan and used without further purification. Ethyl acetate was dried over CaH₂ and distilled before use. Flash column chromatography was performed on 230–400 mesh SiO₂ gel (SiliaFlash^® P60, 40–63 μm 60 Å; SiliCycle^® Inc., Quebec City, QC, Canada). Structural determinations were based on ¹H and ¹³C nuclear magnetic resonance spectroscopy (NMR) data and were recorded on a Bruker 600 MHz Ultrashield instrument. The chemical shifts were reported in parts per million (ppm) relative to the residual of the solvents: ¹H (7.26 ppm) and ¹³C (77.0 ppm) for CDCl₃, and ¹H (4.78 ppm) and ¹³C (49.15 ppm) for CD₃OD. Melting points were measured using an MP-2D apparatus and were uncorrected. The molecular weights of the compounds were determined by high-resolution mass spectrometry (HRMS) using a TMS-700 instrument in the electrospray ionization (ESI) mode. MS 4 Å was oven-dried overnight at 100 °C before use.

Cheng Y.J., Li C.W., Kuo C.L., Shih T.L, & Chen J.J. (2022). Improved Synthesis of Asymmetric Curcuminoids and Their Assessment as Antioxidants. Molecules, 27(8), 2547.

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Fractionation of R. subarcticum Essential Oil

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Fractionation of R. subarcticum essential oil was done by flash chromatography
on a silica gel column (Silicycle, SiliaFlash P60, 40–63 μm)
using a hexanes/methylene chloride (both purified using the VAC 103991
solvent purification system) gradient (50 mL each: 90/10, 70/30, 50/50,
20/80, and 0/100). The essential oil (500 mg) was fractionated on
a 30 g silica gel column, and fractions were collected in 5 mL volumes.
Fractions 25–31 contained over 90% ascaridole, as determined
by GC/FID.

Séguin J.C., Gagnon D., Bélanger S., Richard D., Fernandez X., Boudreau S, & Voyer N. (2023). Chemical Composition and Antiplasmodial Activity of the Essential Oil of Rhododendron subarcticum Leaves from Nunavik, Québec, Canada. ACS Omega, 8(19), 16729-16737.

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Antioxidant Capacity of Horseshoe Crab

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Horseshoe crab (Tachypleus tridentatus) was collected from the North Gulf, Xiamen, China. Reversed phase silica gel YMC-ODS C18 was purchased from YMC (Kyoto, Japan). Silica gel chromatography plates GF254 were obtained from Qingdao Ocean Chemical Plant (Qingdao, China). We prepared normal phase column chromatography silica gel (Silia Flash P60) from SiliCycle (Quebec City, Canada), Sephadex LH-20 from GE Healthcare (Uppsala, Sweden), and deuterated solvents for NMR experiments from Shanghai Macklin Biochemical Co. Ltd. (Shanghai, China). Methanoic acid and methanol for ESI-MS were purchased from TEDIA Biochemical Co. Ltd. (USA). For FRAP and ABTS assay, we used total antioxidant capacity assay kit from Beyotime Institute of Biotechnology (Shanghai, China). We acquired all other reagents with analytical grade from Sinopharm Chemical Reagent Co. (Shanghai, China).

Li J., Zhang Y., Yang S., Lu Z., Li G., Wu S., Wu D.R., Liu J., Zhou B., Wang H.M, & Huang S.Y. (2021). The Beneficial Effects of Edible Kynurenic Acid from Marine Horseshoe Crab (Tachypleus tridentatus) on Obesity, Hyperlipidemia, and Gut Microbiota in High-Fat Diet-Fed Mice. Oxidative Medicine and Cellular Longevity, 2021, 8874503.

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NMR Spectroscopy and Chromatography Analysis

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All chemicals were purchased from Sigma-Aldrich (Shanghai, China) or Alfa-Aesar (Heysham, Lancashire, UK) companies and used without further purification. ¹H and ¹³C NMR data were recorded on a Bruker 600 Ultrashield NMR spectrophotometer (Bruker, New Taipei City, Taiwan). The chemical shifts were reported in part per million (ppm) with the designated deuterium solvent relative to the residual solvent as internal standard (CDCl₃, ¹H: 7.26 ppm; ¹³C: 77.0 ppm.; CD₃OD, ¹H: 4.78 ppm; ¹³C: 49.15 ppm). Purification by flash column chromatography (SiliaFlash^® P60, 40–63 μm 60Å, SiliCycle^® Inc., Quebec City, QC, Canada) was performed on 230–400 mesh SiO₂. The melting points were measured by a MP-2D apparatus (Fargo, New Taipei City, Taiwan) and not corrected. The mass data were obtained from JEOL JNS-700 (Akishima, Tokyo, Japan) by either EI or FAB and Bruker UltraFlex II for ESI (Bruker, New Taipei City, Taiwan).

Hung S.J., Hong Y.A., Lin K.Y., Hua Y.W., Kuo C.J., Hu A., Shih T.L, & Chen H.P. (2020). Efficient Photodynamic Killing of Gram-Positive Bacteria by Synthetic Curcuminoids. International Journal of Molecular Sciences, 21(23), 9024.

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Synthesis of Explosive Peroxide Intermediates

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All commercially available compounds were purchased and used as received, unless otherwise noted. Anhydrous 1,4-dioxane in 100 ml sure-seal bottles was purchased from Aldrich. ¹H and ¹³C NMR spectra were recorded on Bruker 400 MHz or 500 MHz spectrometers and chemical shifts are given in parts per million relative to internal tetramethylsilane (0.00 ppm for ¹H) or CDCl₃ (77.16 ppm for ¹³C). Flash chromatography was carried out with SiliaFlash® P60 (Silicycle, particle size 40–63 um, 2300–400 mesh) or by using a CombiFlash Rf® automated chromatography system with reusable high performance silica columns (RediSep® Rf Gold Silica, 200–40 µm spherical particles).
CAUTION: Although no explosions or other safety incidents were encountered in the course of this work, the experiments described here involve the formation of potentially explosive peroxide intermediates. All reactions were performed on small scale behind a blast shield. Appropriate safety measures should be taken into consideration in the reproduction or extension of this work.

Weinstein A.B, & Stahl S.S. (2014). Palladium Catalyzed Aryl C–H Amination with O2 via In Situ Formation of Peroxide-Based Oxidant(s) from Dioxane. Catalysis science & technology, 4(12), 4301-4307.

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Analytical Characterization of Organic Compounds

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¹H and ¹³C NMR spectra
were recorded on a Varian Mercury-300 NMR spectrometer or a Bruker
AVANCE III HD NanoBay 400 MHz spectrometer, and chemical shifts were
measured in ppm relative to the specific solvent signal. Routine mass
and purity analyses (LRMS) were performed on an HP Agilent LC/MS series
1100 system equipped with a reverse phase column (Agilent Poroshell
120 EC-C18, 2.7 μm, 50 × 2.1 mm) and photodiode array detector
coupled to an Agilent 1946 DSL quadrupole mass selective detector
using electrospray ionization (ESI). The gradient mobile phase consisting
of acetonitrile/water with 0.1% formic acid and UV detection at 254
and 210 nm were used to confirm all final products to be ≥95%.
The melting point was measured on an Electrothermal 9100 apparatus.
Most reagents used in the synthetic procedure were purchased from
Sigma-Aldrich, Alfa Aesar, and TCI. The progress of the reaction was
monitored using thin-layer chromatography (TLC) (silica gel 60 F254
0.25 mm), and the products were visualized by UV light (254 and 365
nm). SiliaFlash P60 (40–60 μm) used in flash column chromatography
was purchased from Silicycle Inc. Other solvents were purchased from
commercial vendors and used without further purification unless otherwise
mentioned.

Oh S., Libardo M.D., Azeeza S., Pauly G.T., Roma J.S., Sajid A., Tateishi Y., Duncombe C., Goodwin M., Ioerger T.R., Wyatt P.G., Ray P.C., Gray D.W., Boshoff H.I, & Barry CE I.I.I. (2021). Structure–Activity Relationships of Pyrazolo[1,5-a]pyrimidin-7(4H)-ones as Antitubercular Agents. ACS Infectious Diseases, 7(2), 479-492.

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Improved Pulegone Bishydroxylation Separation

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Example 1

Both the selectivity and yields obtained for the α,α′-bishydroxylation of pulegone can depend on the quality of KHMDS and control of the temperature. Separation of the diastereomeric products was improved via use of wet silica gel, prepared as follows: Silica gel (SiliaFlash® P60, particle size 40-63 microns [230 to 400 mesh], purchased from Silicycle, 950 g) was slowly mixed with deionized water (50 mL) in a 1-liter media bottle. The silica was then vigorously shaken for five minutes, and then allowed to equilibrate for 12 h before use as normal for silica gel purification. The product obtained by this method was typically 97% pure by ₁H NMR analysis, containing some minor oxaziridine-derived products.

US10392360B2. Synthetic route to anhydroryanodol, ryanodol and structural analogues (2019-08-27). California Institute of Technology [US]. Inventors: Sarah Reisman [US], Kangway V. Chuang [US], Chen Xu [US].

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Non-Aqueous Reaction Procedures

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All non-aqueous reactions were carried out under a dry N₂ atmosphere with oven-dried (115 °C) glassware. All solvents and reagents were of reagent quality, purchased commercially, and used without further purification unless otherwise indicated. Reactions were monitored by thin layer chromatography using EMD pre-coated silica gel 60 F₂₅₄ plates. Flash chromatography was carried out using Silicycle SiliaFlash P60 (230–400 mesh) silica gel. Unless otherwise noted, ¹H and ¹³C NMR spectra were recorded on a 500 MHz Varian Unity Inova spectrometer. All NMR measurements were carried out in DMSO-d₆ at ambient temperature. Chemical shifts are in parts per million (ppm), relative to the residual peaks of DMSO-d₆ (¹H: 2.50; ¹³C: 39.52). Coupling constants (J) were reported in Hertz. Low resolution electrospray ionization mass spectra (LR-ESI-MS) were obtained by the Mass Spectrometry Laboratory, School of Chemical Sciences, University of Illinois at Urbana-Champaign.

Luu L.M., Nguyen L., Peng S., Lee J., Lee H.Y., Wong C.H., Hergenrother P.J., Chan H.Y, & Zimmerman S.C. (2016). A Potent Inhibitor of Protein Sequestration by Expanded Triplet (CUG) Repeats that Shows Phenotypic Improvements in a Drosophila Model of Myotonic Dystrophy. ChemMedChem, 11(13), 1428-1435.

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