Isco combiflash rf

Manufactured by Teledyne

Sourced in United States

The ISCO CombiFlash Rf is a flash chromatography system designed for purification and isolation of compounds. It features automated solvent delivery, fraction collection, and detection capabilities to streamline the purification process.

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ISCO CombiFlash Rf system ISCO-CombiFlash® Rf 200 Combiflash ISCO Combiflash Rf CombiFlash

10 protocols using isco combiflash rf

Analytical Characterization of Compounds

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NMR data were collected using a JEOL ECA-500 NMR spectrometer operating at 500 MHz for ¹H and 125 MHz for ¹³C (JEOL Ltd., Tokyo, Japan). Residual solvent signals were utilized for referencing. High resolution mass spectra (HRMS) were obtained using a Thermo LTQ Orbitrap XL mass spectrometer equipped with an electrospray ionization source (Thermo Fisher Scientific, San Jose, CA, USA). Phenomenex Gemini-NX C₁₈ analytical (5 μm; 250 × 4.6 mm) and preparative (5 μm; 250 × 21.2 mm) columns (Phenomenex, Torrance, CA, USA) were used on a Varian Prostar HPLC system equipped with Prostar 210 pumps and a Prostar 335 photodiode array detector (PDA), with data collected and analyzed using Galaxie Chromatography Workstation software (version1.9.3.2, Varian Inc.). Flash chromatography was conducted on a Teledyne ISCO CombiFlash Rf using Silica Gold columns and monitored by UV and evaporative light-scattering detectors (both from Teledyne Isco, Lincoln, NE, USA).

Parlet C.P., Kavanaugh J.S., Crosby H.A., Raja H.A., El-Elimat T., Todd D.A., Pearce C.J., Cech N.B., Oberlies N.H, & Horswill A.R. (2019). Apicidin Attenuates MRSA Virulence through Quorum-Sensing Inhibition and Enhanced Host Defense. Cell reports, 27(1), 187-198.e6.

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Melting Point and Chromatographic Analysis

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Melting points were determined on a Thomas-Hoover capillary tube apparatus. Thin layer chromatography was carried out using Merck Silica Gel 60F254 TLC plates; visualization was under UV. High pressure liquid chromatography was carried out on a system comprised of two Rainin Dynamax Pumps Model SD-300 equipped with a Rheodyne Model 7725i Injector, and a Varian ProStar 330 Detector; the system was controlled using Varian Star Version 5.5.
Chromatographic purification was performed on a Teledyne ISCO CombiFlash Rf. Nuclear magnetic resonance (NMR) spectra were recorded on a Bruker Avance 300 MHz or a Varian Unity Inova 500 MHz NMR spectrometer. Microanalyses were performed by Atlantic Microlab, Inc. X-ray diffraction analysis was carried out by the Naval Research Laboratory.

McElhinny C.J., Lewin A.H., Brieaddy L., Fix S., Imler G.H., Deschamps J., Mascarella S.W., Seltzman H.H., Reddy P.A, & Carroll F.I. (2021). α-[Amino(4-aminophenyl)thio]methylene-2-(trifluoromethyl)benzeneacetonitrile; Configurational Equilibria in Solution. Bioorganic chemistry, 113, 104955.

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Analytical Thin-Layer Chromatography and Flash Column Purification

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Analytical thin-layer chromatography was performed using Sorbent Technologies 250 μm glass-backed UV254 silica gel plates. The plates were first visualized by means of fluorescence upon 254 nm irradiation then using an iodine chamber and subsequently with phosphomolybdic acid with heating. Flash column chromatography was performed using Sorbent Technologies 40–63 μm, pore size 60 Å silica gel in Luknova columns on a Teledyne ISCO CombiFlash Rf with solvent systems indicated. Solvent removal was effected using a Buchi R3 rotary evaporator with a V900 diaphragm pump (~10 mmHg). Further drying of samples was conducted using a Welch vacuum pump at <0 mmHg. All isolated yields refer to material that is chromatographically (TLC or HPLC) and spectroscopically (¹H NMR) homogenous.

Donahue M.G, & Crull E. (2023). (R)-(+)-3,5-Dinitro-N-(1-phenylethyl)benzothioamide. Molbank, 2023(2), M1650.

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Optimized Synthetic Reactions Protocol

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All synthetic reactions were
carried out in oven-dried vessels under a dry N₂ atmosphere.
All chemicals were obtained from commercial sources and used as received.
THF was freshly distilled over Na/benzophenone prior to use. CDCl₃ and DMF were dried using molecular sieves (3 and 4 Å,
respectively). Microwave heating was performed using sealed flasks
on a CEM Discover System 908010. Automated flash column chromatography
was performed on a Teledyne ISCO CombiFlash Rf⁺ Lumen automated
flash chromatography System with UV/vis detection. ¹H, ¹³C, and ¹⁹F NMR spectra were measured at ambient
temperature using 5 mm diameter NMR tubes. The chemical shift values
(δ) are reported in ppm relative to internal Me₄Si
(0 ppm for ¹H and ¹³C NMR) or residual solvents
and internal CFCl₃ (0 ppm for ¹⁹F NMR). High-resolution
MS spectra (HRMS) were recorded on an LTQ Orbitrap XL using electrospray
(ESI) or APCI ionization on a Waters Micromass AutoSpec Ultima or
Agilent 7890A GC coupled with Waters GCT Premier orthogonal acceleration
TOF detector using electron impact (EI) or chemical ionization (CI).
Simultaneous thermogravimetric and differential scan calorimetry (TG-DSC)
was carried out using a Setaram Sensys Evo thermal analyzer equipped
with a symmetrical balance and a Calvet 3D sensor.

Ziabko M., Klepetářová B, & Beier P. (2023). Synthesis of Azidodifluoromethyl Phenyl Sulfone and Its Use as a Synthetic Equivalent of the Azidodifluoromethyl Anion. The Journal of Organic Chemistry, 88(11), 6939-6946.

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Characterization of Synthetic Organic Compounds

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Reagents were purchased from Sigma-Aldrich, TCI, and Acros and were used without further purification unless otherwise specified. Solvents were purchased from Sigma-Aldrich and Fisher Scientific, and dried by standard techniques. NMR solvents were purchased from Cambridge Isotope Laboratories (Andover, MA). All reactions were monitored with analytical TLC (Merck Kieselgel 60 F₂₅₄). Column chromatography was carried out with Teledyne ISCO Combiflash Rf with silica gel particle size 40–63 um. NMR spectra were obtained on Varian Mercury 300 MHz and Varian VX 500 MHz. Mass spectra were obtained on an Agilent 6230 HR-ESI-TOF MS at the Mass Spectrometry Facility at the UCSD Chemistry and Biochemistry Department.

Ludford PT I.I.I., Rovira A.R., Fin A, & Tor Y. (2019). Fluorescing Isofunctional Ribonucleosides: Assessing Adenosine Deaminase Activity and Inhibition. Chembiochem : a European journal of chemical biology, 20(5), 718-726.

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Characterization of Organic Compounds via Spectroscopic Techniques

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Chemical reagents purchased from commercial suppliers were not further purified prior to use. Flash column chromatography was performed using silica gel (4-63 mm) purchased from Sorbent Technologies. Other chemical separations were performed using a Teledyne Isco CombiFlash Rf. A Biotage microwave reactor was used when microwaving was necessary. ¹H and ¹³C NMR were recorded using a 500 MHz Bruker AVIII spectrometer equipped with a cryogenically-cooled carbon observe probe. Tetramethylsilane was used as an internal standard and chemical shifts (δ) are reported in ppm and coupling constants (J) are reported in Hz. High-resolution mass spectrometry (HRMS) was performed using an electrospray ion source in either positive or negative mode on an LCT Premier (Micromass Ltd., Manchester UK). Melting points were measured with a Thomas Capillary Melting Point Apparatus and are uncorrected. Chiral analysis was carried out using HPLC, 1 ml/min hexane:isopropanol (90:10) on a CHIRALCEL® OD-H column, monitored at 320 nm unless otherwise specified.

Ronnebaum T.A., McFarlane J.S., Prisinzano T.E., Booker S.J, & Lamb A.L. (2018). Stuffed Methyltransferase Catalyzes Penultimate Step of Pyochelin Biosynthesis. Biochemistry, 58(6), 665-678.

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Analytical Techniques for Compound Characterization

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All reagents were used in the condition received from commercial sources. ¹H NMR and ¹³C NMR were taken in CDCl₃ or DMSO-d₆ at room temperature on Varian Inova 400 or 500 MHz instruments. Reported chemical shifts are expressed in parts per million (ppm) on the δ scale from an internal standard of tetramethylsilane (0 ppm). Mass spectrometry data were obtained on either an Agilent TOF or Agilent Q-TOF. An Agilent 1100 series HPLC with an Agilent Zorbax Eclipse Plus−C18 column was used to determine purity of biologically tested compounds. All tested compounds were determined to be >95% pure using a 6 minute gradient of 10–90% acetonitrile in water followed by a 2 minute hold at 90% acetonitrile with detection at 254 nm. Flash chromatographic purifications were performed using a Teledyne ISCO Combiflash RF with Redisep Gold RF columns.

Huddle B.C., Grimley E., Buchman C.D., Chtcherbinine M., Debnath B., Mehta P., Yang K., Morgan C.A., Li S., Felton J., Sun D., Mehta G., Neamati N., Buckanovich R.J., Hurley T.D, & Larsen S.D. (2018). Structure-Based Optimization of a Novel Class of Aldehyde Dehydrogenase 1A (ALDH1A) Subfamily-Selective Inhibitors as Potential Adjuncts to Ovarian Cancer Chemotherapy. Journal of medicinal chemistry, 61(19), 8754-8773.

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Purification and Characterization Protocol

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All reagents were used in the condition received from commercial sources. Flash chromatographic purifications were performed using a Teledyne ISCO Combiflash RF with Redisep Gold RF silica columns. ¹H NMR and ¹³C NMR were taken in CDCl₃ or DMSO-d6 at room temperature on Varian Inova 400 or 500 MHz instruments. Reported chemical shifts are expressed in parts per million (ppm) on the δ scale from an internal standard of tetramethylsilane (0 ppm). Mass spectrometry data were obtained on either an Agilent TOF or Agilent Q-TOF. An Agilent 1100 series HPLC with an Agilent Zorbax Eclipse Plus-C18 column was used to determine purity of biologically tested compounds. All tested compounds were determined to be >95% pure using a 6 min gradient of 10-90% acetonitrile in water followed by a 2 min hold at 90% acetonitrile with detection at 254 nm. Enantiomeric excesses were determined by chiral analytical HPLC using a Daicel Chiralcel OD column 4.6X250mm. Optical rotations were determined by Robertson Microlit Laboratories (http://www.robertson-microlit.com) according to USP <781S> protocol.
NCT-506 used as a comparator in biological studies was prepared as described by Yang et al.^{36 (link)}

Huddle B.C., Grimley E., Chtcherbinine M., Buchman C.D., Takahashi C., Debnath B., McGonigal S.C., Mao S., Li S., Felton J., Pan S., Wen B., Sun D., Neamati N., Buckanovich R.J., Hurley T.D, & Larsen S.D. (2020). Development of 2,5-dihydro-4H-pyrazolo[3,4-d]pyrimidin-4-one inhibitors of Aldehyde Dehydrogenase 1A (ALDH1A) as potential adjuncts to ovarian cancer chemotherapy. European journal of medicinal chemistry, 211, 113060.

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Characterization of Organic Compounds

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All reagents were used without further purification as received from commercial sources unless noted otherwise. ¹H NMR spectra were taken in DMSO-d6, MeOD, or CDCl₃ at room temperature on Varian Inova 400 MHz or Varian Inova 500 MHz instruments. Reported chemical shifts for the ¹H NMR and ¹³C NMR spectra were recorded in parts per million (ppm) on the δ scale from an internal standard of residual tetramethylsilane (0 ppm). Mass spectrometry data were obtained on either a Micromass LCT or Agilent Q-TOF. An Agilent 1100 series HPLC with an Agilent Zorbax Eclipse Plus–C18 column was used to determine purity of biologically tested compounds. Unless otherwise noted, all tested compounds were determined to be >95% pure using a 6 minute gradient of 10–90% acetonitrile in water followed by a 2 minute hold at 90% acetonitrile with detection at 254 nm. Flash chromatographic purifications were performed using a Teledyne ISCO Combiflash RF with Redisep Gold RF columns.

Zwicker J.D., Smith D., Guerra A.J., Hitchens J.R., Haug N., Vander Roest S., Lee P., Wen B., Sun D., Wang L., Keep R.F., Xiang J., Carruthers V.B, & Larsen S.D. (2020). Discovery and Optimization of Triazine Nitrile Inhibitors of Toxoplasma gondii Cathepsin L for the Potential Treatment of Chronic Toxoplasmosis in the CNS. ACS chemical neuroscience, 11(16), 2450-2463.

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Synthesis and Purification of Venglustat

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All reagents and solvents were used in the condition received from commercial sources. Chromatographic purifications were performed using a Teledyne ISCO Combiflash RF with Redisep columns or by standard flash chromatography using silica gel (220−240 mesh) obtained from Silicycle. ¹H NMR were taken in CDCl₃ or DMSO-d₆ at room temperature on Varian Inova 400 or 500 MHz instruments. Reported chemical shifts are expressed in parts per million (ppm) on the δ scale from an internal standard of tetramethylsilane (0 ppm). Mass spectra were recorded on a Micromass LCT time-of-flight instrument utilizing the electrospray ionization mode. An Agilent 1100 series HPLC with an Agilent Zorbax Eclipse Plus−C18 column (3.5 um, 4.6 × 100 mm) was used to determine “HPLC purity” of biologically tested compounds. All tested compounds were assayed for purity using a 6 min gradient of 10−90% acetonitrile in water followed by a 2 min hold at 90% acetonitrile with detection at 254 nm.
Eliglustat tartrate used in these studies was obtained from Genzyme Corporation. Genz-682452 (3, venglustat) was prepared by the method described by Zhao et al.¹⁹

Wilson M.W., Shu L., Hinkovska-Galcheva V., Jin Y., Rajeswaran W., Abe A., Zhao T., Luo R., Wang L., Wen B., Liou B., Fannin V., Sun D., Sun Y., Shayman J.A, & Larsen S.D. (2020). Optimization of Eliglustat-Based Glucosylceramide Synthase Inhibitors as Substrate Reduction Therapy for Gaucher Disease Type 3. ACS chemical neuroscience, 11(20), 3464-3473.

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