Solvents were purified by standard methods.[16] Palladium(II) acetate, Thallium(I) acetylacetonate, (p‐NH2C6H4)2SO2, (p‐NH2C6H4)2O, (p‐NH2C6H4)2CH2, and the phosphines P(pMeOPh)3, P(pMePh)3, Ph2PCH2PPh2 (dppm) and Ph2P(CH2)3PPh2 (dppp) were purchased from commercial sources; Ph2PN(Me)PPh2 (dppma), personal loan to Professor JM Vila. Elemental analyses were performed with a Fisons elemental analyzer, Model 1108. IR spectra were recorded on BRUKER FT‐MIR model VERTEX 70 V, and Jasco model FT/IR‐4600 spectrophotometers. 1H NMR spectra in solution were recorded in CDCl3, DMSO‐d6, CD2Cl2, or (CD3)2CO at room temperature on Bruker DPX 250 and Varian Inova 400 spectrometers operating at 250.13 MHz and 400.14 MHz respectively and using 5 mm o.d. tubes; chemical shifts, in ppm, are reported downfield relative to TMS using the solvent signal (CDCl3, δ1H=7.26 ppm; DMSO‐d6, δ1H=2.50 ppm; CD2Cl2 d6 δ1H=5.32 ppm, MeCOMe‐d6 δ1H=2.05 ppm) as reference. 31P NMR spectra were recorded at 161.91 MHz and on a Varian Inova 400 spectrometer using 5 mm o.d. tubes and are reported in ppm relative to external H3PO4 (85 %). Coupling constants are reported in Hz.
Inova 400
Manufactured by Agilent Technologies
Sourced in United States
The Inova 400 is a nuclear magnetic resonance (NMR) spectrometer designed for analytical chemistry applications. It provides a magnetic field strength of 9.4 Tesla and operates at a 1H frequency of 400 MHz. The Inova 400 is capable of performing various NMR experiments to analyze the structure and composition of chemical samples.
Automatically generated - may contain errors
Lab products found in correlation
Inova 500, by Agilent Technologies (4 mentions)
Inova 600, by Agilent Technologies (4 mentions)
Silica gel 60 f254 plate, by Merck Group (3 mentions)
241 polarimeter, by PerkinElmer (3 mentions)
Isco combiflash rf, by Teledyne (3 mentions)
Zorbax eclipse plus c18 column, by Agilent Technologies (3 mentions)
Silica gel 60 f254, by Merck Group (2 mentions)
1100 series instrument, by Hewlett-Packard (2 mentions)
Mercury 300, by Agilent Technologies (2 mentions)
Mercury plus 400, by Agilent Technologies (2 mentions)
Avance dpx 200, by Bruker (2 mentions)
Mercury 300 mhz, by Agilent Technologies (2 mentions)
Cdcl3, by Cambridge Isotopes (2 mentions)
Cd3od, by Cambridge Isotopes (2 mentions)
Gemini 300, by Agilent Technologies (2 mentions)
Dimethyl sulfoxide (dmso), by Merck Group (2 mentions)
Silica gel, by Qingdao Marine Chemical (2 mentions)
Agilent 1260 hplc, by Agilent Technologies (1 mentions)
500 spectrometers, by Agilent Technologies (1 mentions)
Anhydrous dmf, by Thermo Fisher Scientific (1 mentions)
65 protocols using inova 400
1
Purification and Characterization of Organometallic Compounds
2
NMR Spectroscopy Data Acquisition Protocol
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1H-NMR spectra: Bruker Avance III (400 MHz) and Varian INOVA 400 (400 MHz). 1H chemical shifts are reported in ppm relative to residual peaks of deuterated solvents. The observed signal multiplicities are characterized as follows: s = singlet, d = doublet, t = triplet, m = multiplet, and br = broad. Coupling constants (J) were reported in Hertz (Hz). 13C-NMR spectra [additional APT (Attached Proton Test) or DEPT (Distortionless Enhancement by Polarization Transfer)]: Bruker Avance III (101 MHz) and Varian INOVA 400 (101 MHz). 13C chemical shifts are reported in ppm relative to residual peaks of deuterated solvents. 19F-NMR spectra: and Bruker DPX Avance 200 (188 MHz). Copies of the 1H and 13C NMR spectra are available in the Supplementary Materials .
3
Synthetic Methodology for Neomycin B and Kanamycin A
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All reactions were carried out in oven-dried glassware under a positive pressure of argon unless otherwise noted. Neomycin B and Kanamycin A free bases were prepared from the corresponding monosulfate salts (purchased from Santa Cruz Biotechnology, inc. and Sigma-Aldrich, respectively) by use of Amberlite-IRA 400 (OH−) strongly basic ion-exchange resin. Solvents were dried in a Pure Solv system model PS-400-3-MD. Reactions were monitored by analytical thin-layer chromatography (TLC) on EM silica gel 60 F254 plates (0.25 mm), visualized by ultraviolet light and/or by staining with ceric ammonium molybdate, H2SO4 or ninhydrin. Column chromatography was performed on Silice 60 (230–400 µM) and on Amberlite CG-50 (NH4+) cation exchange resin. 1H NMR spectra were recorded on a Varian Inova-400 (400 MHz) and Varian UNITY 500 (500 MHz) in CDCl3, CD3OD and D2O solutions at ambient temperature. Data were reported as follows: chemical shift on the δ scale (either using TMS or residual proton solvent as internal standard), multiplicity (br = broad, s = singlet, d = doublet, t = triplet, q = quartet, m = multiplet), coupling constant(s) in hertz, and integration. 13C NMR spectra were recorded on a Varian Inova-400 (100 MHz) and Varian UNITY 500 (125 MHz). Mass spectra were recorded on an AGILENT 6520 Accurate-Mass QTOF LC/MS spectrometer using the electrospray modes (ES).
4
NMR Spectroscopic Analysis Protocols
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1H-NMR spectra: Bruker DPX Avance 200 (200 MHz), Bruker Avance II 300 (300 MHz) and Varian INOVA 400 (400 MHz). 1H chemical shifts are reported in ppm relative to residual peaks of deuterated solvents. The observed signal multiplicities are characterized as follows: s = singlet, d = doublet, t = triplet, m = multiplet, and br = broad. Coupling constants (J) were reported in Hertz (Hz). 13C-NMR spectra [additional APT (Attached Proton Test)]: Bruker DPX Avance 200 (50 MHz), Bruker Avance II 300 (75 MHz) and Varian INOVA 400 (101 MHz). 13C chemical shifts are reported in ppm relative to residual peaks of deuterated solvents.
19F-NMR spectra: Bruker DPX Avance 200 (188 MHz).
19F-NMR spectra: Bruker DPX Avance 200 (188 MHz).
5
General Analytical Procedures and Characterization
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General. Analytical grade solvents and commercially available reagents were used without further purification. Reactions requiring inert atmosphere were carried out under argon atmosphere. Flash chromatography was performed using 32-63 μm silica gel (60 Å mesh) with the indicated solvent.
Analytical thin layer chromatography (TLC) was performed on 0.25 mm silica gel 60-F plates. Melting points were determined with a BÜCHI B-540 instrument and are uncorrected. Optical rotation measurements were performed on a JASCO DIP-370 polarimeter. 1 H NMR spectra were acquired on Varian INOVA-400 and on Varian MercuryPlus-400 spectrometers. 13 C NMR spectra were acquired on Varian INOVA-400, Varian MercuryPlus-400 spectrometers running at 100 MHz, and on Varian Gemini-200 spectrometer, running at 50 MHz. All chemical shifts are reported in parts per million (δ) referenced to residual nondeuterated solvent. Data are reported as follows: chemical shifts, multiplicity (br = broad, s = singlet, d = doublet, t = triplet, q = quartet, m = multiplet; coupling constant(s) in Hz; integration). ESI mass spectra were carried out on a ion-trap double quadrupole mass spectrometer using electrospray (ES + ) ionization techniques, and a normalized collision energy within the range of 25-32 eV for MSMS experiments. Elemental analyses were performed with a Perkin-Elmer 2400 analyzer.
Analytical thin layer chromatography (TLC) was performed on 0.25 mm silica gel 60-F plates. Melting points were determined with a BÜCHI B-540 instrument and are uncorrected. Optical rotation measurements were performed on a JASCO DIP-370 polarimeter. 1 H NMR spectra were acquired on Varian INOVA-400 and on Varian MercuryPlus-400 spectrometers. 13 C NMR spectra were acquired on Varian INOVA-400, Varian MercuryPlus-400 spectrometers running at 100 MHz, and on Varian Gemini-200 spectrometer, running at 50 MHz. All chemical shifts are reported in parts per million (δ) referenced to residual nondeuterated solvent. Data are reported as follows: chemical shifts, multiplicity (br = broad, s = singlet, d = doublet, t = triplet, q = quartet, m = multiplet; coupling constant(s) in Hz; integration). ESI mass spectra were carried out on a ion-trap double quadrupole mass spectrometer using electrospray (ES + ) ionization techniques, and a normalized collision energy within the range of 25-32 eV for MSMS experiments. Elemental analyses were performed with a Perkin-Elmer 2400 analyzer.
6
Synthesis and Characterization of a Bimetallic PtIr Complex
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The syntheses were carried out using standard Schlenk techniques under an atmosphere of nitrogen. The complex [PtIr-(CO) 3 (μ-dppm) 2 ][PF 6 ], 1, was prepared by the literature method, from [Pt(η 2 -dppm) 2 ][PF 6 ] 2 and [PPN][Ir(CO) 4 ], and 13 CO enriched samples were prepared by stirring under an atmosphere of 13 CO. 6, 28 The 1 H, 31 P{ 1 H}, and 13 C{ 1 H} NMR spectra were recorded using a Varian Gemini 300, Varian Inova 400 or Inova 600 spectrometer. The gCOSY, gHSQC, and gHMBC spectra were recorded using the Varian Inova 400 or Inova 600 spectrometer. Chemical shifts are cited with respect to TMS or 85% phosphoric acid ( 31 P). IR spectra were recorded with Nujol mulls or solutions using a Perkin Elmer 2000 FTIR spectrometer. Emission spectra were recorded by using a Fluorolog-3 spectrofluorimeter (ISA Jobin Yvon Spex), using a solution in CH 2 Cl 2 at room temperature in a quartz cuvette. DFT calculations (gas phase only) were carried out by using the Amsterdam Density Functional (ADF) program based on the BP functional, with double-zeta basis set and first-order scalar relativistic corrections. 26
7
High-Purity Compound Screening and Synthesis
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All experimental compounds for initial screening were purchased from Asinex (Winston-Salem, NC, USA) or synthesized in house. Purities were required to be greater than 90% with a majority of commercial compounds having a purity of greater than 95%. Compounds were all dissolved in dimethyl sulfoxide (Sigma Aldrich) at a stock concentration of 8.0 mg/mL immediately and then diluted for biological testing.
All reagents for chemical synthesis were purchased from commercial suppliers and used without further purification unless noted otherwise. All chemical reactions occurring solely in an organic solvent were carried out under an inert atmosphere of argon or nitrogen. Analytical TLC was performed with Merck silica gel 60 F254 plates. Silica gel column chromatography was conducted with Teledyne Isco CombiFlash Companion or Rf+ systems. 1H NMR spectra were acquired on Varian Inova 400, 500 and 600 MHz instruments and are listed in parts per million downfield from TMS. LC-MS was performed on an Agilent 1260 HPLC coupled to an Agilent 6120 MS. All synthesized compounds were at least 95% pure as judged by their HPLC trace at 250 nm and were characterized by the expected parent ion(s) in the MS trace. The Supplementary Materials include synthetic details pertinent to the arylamide and quinoxaline di-N-oxide series.
All reagents for chemical synthesis were purchased from commercial suppliers and used without further purification unless noted otherwise. All chemical reactions occurring solely in an organic solvent were carried out under an inert atmosphere of argon or nitrogen. Analytical TLC was performed with Merck silica gel 60 F254 plates. Silica gel column chromatography was conducted with Teledyne Isco CombiFlash Companion or Rf+ systems. 1H NMR spectra were acquired on Varian Inova 400, 500 and 600 MHz instruments and are listed in parts per million downfield from TMS. LC-MS was performed on an Agilent 1260 HPLC coupled to an Agilent 6120 MS. All synthesized compounds were at least 95% pure as judged by their HPLC trace at 250 nm and were characterized by the expected parent ion(s) in the MS trace. The Supplementary Materials include synthetic details pertinent to the arylamide and quinoxaline di-N-oxide series.
8
Synthesis and Characterization of High-Purity Compounds
9
Preparation and Characterization of Organic Compounds
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Tetrahydrofuran (THF) was dried by distillation from sodium/benzophenone ketyl under argon. Anhydrous MeOH was purchased from Aldrich Chemical (cat. No. 322415) and was used as received. Anhydrous DMF was purchased from Alfa Aesar (cat. No. 43997) and was used as received. All other solvents were obtained from Fisher Scientific (Pittsburgh PA, USA; Optima grade) and were used as received. Mass spectra were recorded as described above. 1H and 13C NMR spectra were recorded on a Varian INOVA-400 (400 and 100.5 MHz respectively) spectrometer (Palo Alto, CA), as CDCl3 solutions unless specified otherwise. 1H NMR chemical shifts are expressed in ppm relative to residual CHCl3 (7.27 ppm). 13C NMR chemical shifts are reported relative to CDCl3 (77.16 ppm). Reactions with air- or water-sensitive reagents were carried out in oven-dried glassware under argon. Crude products were purified by flash column chromatography or vacuum flash chromatography on silica gel.
10
Synthesis and Characterization of Novel Compounds
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