Melting points of compounds (1–3 ) were determined on a Bicote melting point apparatus and are uncorrected. UV-visible spectra were recorded on a Hitachi-U-3200 spectrometer, IR spectra on an FT-IR instrument (Nicolet 380), UV-visible spectra on a Shimadzu spectrometer, and 1H-NMR (500 MHz), 13C-NMR (600 MHz), HMBC (600 MHz) and HSQC (600 MHz spectra on an AVANCE AV-600 Cryoprob NMR instrument in CDCl3. HR-EI-MS spectra were measured on a JEOL JMS 600H mass spectrometer; EI source 70 eV. Normal-phase column chromatography (CC) was performed by using silica gel (Merck). TLC was run on pre-coated aluminum plates with silica gel 60 (F254; Merck).
Jms 600h mass spectrometer
Manufactured by JEOL
Sourced in Japan
The JMS 600H is a high-performance mass spectrometer manufactured by JEOL. It is designed to accurately measure the mass-to-charge ratio of ionized molecules, providing detailed information about their molecular composition. The JMS 600H utilizes advanced technology to deliver precise and reliable results for a variety of analytical applications.
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Lab products found in correlation
Silica gel, by Merck Group (3 mentions)
U 3200 spectrometer, by Hitachi (2 mentions)
Silica gel 60, by Merck Group (2 mentions)
Avance 500, by Bruker (2 mentions)
Avance spectrometer, by Bruker (1 mentions)
Vector 22 ftir, by Bruker (1 mentions)
Buchi m 560, by Büchi (1 mentions)
Smart apex 2 x ray single crystal diffractometer, by Bruker (1 mentions)
Sabouraud dextrose agar, by Merck Group (1 mentions)
Nicolet 380, by Thermo Fisher Scientific (1 mentions)
Acetic acid, by Merck Group (1 mentions)
Uv 240, by Shimadzu (1 mentions)
Cary 630 ftir spectrometer, by Agilent Technologies (1 mentions)
500 mhz nmr spectrometer, by Bruker (1 mentions)
70 230 mesh, by Merck Group (1 mentions)
Microtof q mass spectrometer, by Bruker (1 mentions)
Amazon speed spectrometer, by Bruker (1 mentions)
U 3200, by Hitachi (1 mentions)
8900 ft ir spectrophotometer, by Shimadzu (1 mentions)
Sephadex lh 20, by Cytiva (1 mentions)
8 protocols using jms 600h mass spectrometer
1
Characterization of Novel Compounds
2
Characterization of Mestanolone and Derivatives
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Mestanolone (1) was acquired from Hangzhu Dayangchem (Cat no. 541-11-9, China). Sabouraud dextrose agar (SDA) was purchased from Merck KGaA (Cat no. 146392, Germany). Silica gel precoated TLC plates (PF254, Merck KGaA, Germany) were used for thin layer chromatography; phosphomolybdic acid solution was used as a staining reagent for UV inactive compounds. Silica gel (70–230 mesh, Merck, Germany) was used for column chromatography. Final purification of the compounds was carried out by using recycling preparative HPLC-LC-908 (Japan), equipped with JAIGEL-ODS-L-80 column, with MeOH–H2O as the mobile phase. Melting points were recorded on Buchi M-560 (Buchi, Switzerland) apparatus. Optical rotations were measured on JASCO P-2000 (JASCO, Japan) polarimeter. UV Spectra were recorded on Hitachi U-3200 (Hitachi, Tokyo, Japan) spectrophotometer. IR Spectra were recorded as KBr discs on Bruker Vector 22 FT-IR (Bruker) spectrometer. Electron ionization (EI-MS) and high resolution electron ionization mass spectra (HREI-MS) were recorded on JEOL JMS600H mass spectrometer (JEOL, Japan). 1H-, 13C- and 2D-NMR spectra were recorded on Bruker Avance spectrometers (Bruker, Switzerland) in CD3OD. X-Ray diffraction data of the compound 6 was recorded on Bruker SMART APEX II single-crystal X-ray diffractometer (Germany).
3
Characterization of Diclofenac Sodium Derivative
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Melting points were determined using a Bicote (Biby Scientific Limited) apparatus. UV–visible spectra were recorded on a Hitachi-U-3200 spectrometer, and FT-IR spectra were obtained using a Nicolet 380 instrument from Thermo Scientific. UV–visible spectra were also recorded on a Shimadzu spectrometer. NMR spectra (1H at 600 MHz, 13C at 150 MHz) and HMBC spectra were recorded on an Avance AV-600 Cryoprob NMR instrument in CDCl3. EI-MS measurements were conducted on a JEOL JMS 600H mass spectrometer with an EI source set at 70 eV. Diclofenac sodium was purchased from Suzhou Ausun Chemical Co., Ltd., China. Acetic acid and silica gel 60 (0.063–0.200 mm, 5 × 60 cm) were purchased from Merck (Germany). Normal saline was used as a control in all experiments.
4
Spectroscopic Analysis of Organic Compounds
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Electron impact mass spectrometry (EI-MS) was performed on Jeol JMS-600 H mass spectrometer. The 1H-NMR, 13C-NMR, 1H,1H-COSY 45°, HMBC, HSQC, NOESY spectra were recorded in deuterated CDCl3 on Bruker Avance-500, 400, 300 and 100 MHz instruments. Chemical shift (δ) in ppm and coupling constants (J) are in Hz, related to Tetramethylsilane (TMS) which was used as an internal standard. Ultraviolet (UV) experiments were recorded in spectroscopic grade methanol on a Shimadzu UV 240 (Shimadzu CorporationTokyo, Japan). Infrared (IR) spectra were measured in chloroform, as KBr disc on Shimadzu FT IR-8900 spectrophotometer or JASCO A-302 (JASCO International Co. Ltd., Japan).
5
Synthesis and Characterization of Novel Compounds
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All the chemicals were purchased from Sigma–Aldrich (Riedstraße, Germany), and Fluka (Buchs, Switzerland), and were used without further purification, unless otherwise reported. The melting points were measured on a Gallenkamp melting point apparatus (Bibby Scientific Limited, Beacon Road, Stone, Staffordshire, UK) in open glass capillaries and are not corrected. The infrared (IR) spectra were measured as KBr pellets on a Nicolet 6700 Fourier-transform IR spectrophotometer (Thermo Fisher Scientific, Madison, WI, USA). The 1H (400 MHz) and 13C (100 MHz) nuclear magnetic resonance (NMR) spectra were recorded on a Varian Mercury Jeol-400 NMR spectrometer (Tokyo, Japan) in CDCl3 or DMSO-d6. The chemical shifts (δ) are provided in ppm and the J coupling constants in Hz. The mass spectra were recorded on a JEOL JMS-600 H mass spectrometer (Santa Clara, CA, USA). while the elemental analysis of the synthesized compounds was performed using an Elmer 2400 Elemental Analyzer (CHN mode) (Perkin Elmer, Waltham, MA, USA). The AChE assay and molecular docking protocols are described in the supporting information .
6
Spectroscopic Characterization of Aniline Derivatives
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The IR spectrum of all the compounds was done using Cary 630 FTIR Spectrometer (model-Spectrum 400, USA) between the range 4000-650 cm -1 by direct sampling techniques.
The 1 H and 13 C NMR spectra of the derivatives were recorded using Bruker 500MHz NMR spectrometer using CDCl3 and dimethyl sulphoxide-d6 as solvent and TMS as the internal standard. Gas Chromatographic Mass Spectra were recorded on GC-MS QP 2010 plus using Electron Impact Method. HRMS Mass spectra were recorded on JEOL JMS 600H mass spectrometer operating at an ionization mode FAB. 2,4-difluoroaniline, 4-chloro-3trifluoromethyl aniline and 3-chloro-4-trifluoromethoxy aniline were purchased from Alfa Aesar.
Silica gel (Merck) were of analar grade and used as received. Solvent used for the synthesis was glacial acetic acid and solvents used for elution is double distilled. The Silica gel (100-200 Mesh) used for column chromatography were supplied from Rankem. Embelin was Isolated from Embelia ribes. as per the reported procedure [Srinivas 2010 ].
The 1 H and 13 C NMR spectra of the derivatives were recorded using Bruker 500MHz NMR spectrometer using CDCl3 and dimethyl sulphoxide-d6 as solvent and TMS as the internal standard. Gas Chromatographic Mass Spectra were recorded on GC-MS QP 2010 plus using Electron Impact Method. HRMS Mass spectra were recorded on JEOL JMS 600H mass spectrometer operating at an ionization mode FAB. 2,4-difluoroaniline, 4-chloro-3trifluoromethyl aniline and 3-chloro-4-trifluoromethoxy aniline were purchased from Alfa Aesar.
Silica gel (Merck) were of analar grade and used as received. Solvent used for the synthesis was glacial acetic acid and solvents used for elution is double distilled. The Silica gel (100-200 Mesh) used for column chromatography were supplied from Rankem. Embelin was Isolated from Embelia ribes. as per the reported procedure [Srinivas 2010 ].
7
Spectroscopic Analysis of Organic Compounds
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Optical rotations were measured with a P2000 automatic digital Polarimeter. UV spectra were recorded on a Hitachi U-3200. IR spectra were recorded on a shimadzu 8900 FT-IR spectrophotometer in KBr disks. NMR spectra were recorded on Bruker Avance-400, Avance-500, Avance-600 MHz using TMS as an internal standard, with chemical shifts recorded as δ values. ESI-MS data were obtained on an ion-trap (Amazon speed) spectrometer (Bruker, Germany) . HRESI-MS were performed on a MicrOTOF-Q mass spectrometer (Bruker) . The EI-MS and HREI-MS were measured on a Jeol JMS-600H mass spectrometer.
Preparative HPLC was carried out on a Japan Analytical Instrument with a LC-908 W detector using a sil-d-60-80A. Column (250 × 20 mm, 4µm) for a normal phase and ODS H-80 column for reverse phase. Analytical thin layer chromatography (TLC) was performed on precoated silica gel plates (Merck 60 PF 254 ; 20 × 20; 0.25 mm) . Circular dichroism was performed on a JASCO J-810 CD spectrophotometer. Column chromatography (CC) was carried out on silica gel (70-230 Mesh; Merck), Sephadex LH-20 (40-70 μm, Amersham Biosciences, Sweden), and vacuum liquid chromatography (VLC) was performed using silica gel 60 (0.04-0.063 mm; 500 g; Merck, Darmstadt, Germany).
Preparative HPLC was carried out on a Japan Analytical Instrument with a LC-908 W detector using a sil-d-60-80A. Column (250 × 20 mm, 4µm) for a normal phase and ODS H-80 column for reverse phase. Analytical thin layer chromatography (TLC) was performed on precoated silica gel plates (Merck 60 PF 254 ; 20 × 20; 0.25 mm) . Circular dichroism was performed on a JASCO J-810 CD spectrophotometer. Column chromatography (CC) was carried out on silica gel (70-230 Mesh; Merck), Sephadex LH-20 (40-70 μm, Amersham Biosciences, Sweden), and vacuum liquid chromatography (VLC) was performed using silica gel 60 (0.04-0.063 mm; 500 g; Merck, Darmstadt, Germany).
8
Characterization of Organic Compounds via NMR and Mass Spectrometry
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General NMR spectra were recorded on a JNM-ECP400 spectrometer (JEOL Ltd., Japan). Chemical shifts (δ) are reported in ppm using tetramethylsilane or an undeuterated solvent as internal standards in the deuterated solvent used. Coupling constants (J) are given in Hz. Chemical shift multiplicities are reported as s = singlet, d = doublet, t = triplet, m = multiplet. FAB mass spectra were taken on a JMS-600-H mass spectrometer (JEOL Ltd., Japan). Xenon was used as a bombardment gas, and all analyses were carried out in positive mode with the ionization energy and the accelerating voltage set at 70 eV and 3 kV, respectively. A mixture of dithiothreitol (DTT) and α-thioglycerol (TG) (1 : 1) was used as a liquid matrix. High-resolution electrospray ionization (HR-ESI)-MS were measured on a JEOL Model JMS-T100CS mass spectrometer. All conventional chemicals used in the present study are commercially available and were used as received.
Column chromatography was carried out on silica gel (particle size; 46-50 µm; Fuji Silysia Chemical Ltd.).
Column chromatography was carried out on silica gel (particle size; 46-50 µm; Fuji Silysia Chemical Ltd.).
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