General Remarks All reagents and solvents purchased were of the highest commercial quality and were used without further purification. 1 H-NMR spectra were measured at 400 MHz on a VARIAN 400-MR spectrometer or at 500 MHz on an Agilent INOVA-500 spectrometer, and 13 (link) C-NMR spectra were measured at 100 MHz on a VARIAN 400-MR spectrometer or at 125 MHz on an Agilent INOVA-500 spectrometer. High resolution mass spectra were recorded using a Jeol JMS-T100LP AccuTOF instrument. IR spectra were recorded using a JASCO FT/IR-4700 spectrometer in attenuated total reflection (ATR) mode at room temperature. Silica gel column chromatography was performed using Silica Gel 60 (spherical and neutral; 100 to 210 µm, 37560-79, Kanto Chemical Co., Japan) and the Isolera One flash purification system (Biotage, Sweden). After stirring overnight at reflux temperature, the reaction mixture was concentrated under reduced pressure. The residue was dissolved in AcOEt (60 mL), and the solution was washed with water (40 mL×2) and brine (40 mL). The organic layer was dried over Na 2 SO 4 , filtered, and concentrated under reduced pressure. The resulting residue was purified using the Isolera One system (hexane/ AcOEt) to afford 16 as a yellow oil (4435 mg, 81%).
Inova 500 spectrometer
Manufactured by Agilent Technologies
Sourced in United States
The Inova 500 spectrometer is a nuclear magnetic resonance (NMR) instrument manufactured by Agilent Technologies. It is designed to perform high-resolution NMR spectroscopy analysis on samples. The core function of the Inova 500 is to detect and measure the magnetic properties of atomic nuclei within a sample to provide information about its chemical structure and composition.
Automatically generated - may contain errors
Lab products found in correlation
Vector 22 spectrometer, by Bruker (6 mentions)
Cdcl3, by Cambridge Isotopes (3 mentions)
D12 cyclohexane, by Cambridge Isotopes (3 mentions)
Cylindrical quartz banjo cells, by Hellma (3 mentions)
Zetasizer nano zs90, by Malvern Panalytical (3 mentions)
Q gel 60 f254 plates, by Merck Group (2 mentions)
Kieselgel 60, by Merck Group (2 mentions)
Pack ods a column, by YMC (2 mentions)
Silica gel 60 f254, by Merck Group (2 mentions)
Silica gel, by Merck Group (2 mentions)
Synergy 4 multi mode microplate reader, by Agilent Technologies (2 mentions)
Calibur flow cytometer, by BD (2 mentions)
Gpc system, by Malvern Panalytical (2 mentions)
Esi interface, by Shimadzu (2 mentions)
Silica gel, by Qingdao Marine Chemical (2 mentions)
Uv 2450 spectrophotometer, by Shimadzu (2 mentions)
Unity 400 spectrometer, by Agilent Technologies (2 mentions)
P 1020 polarimeter, by Jasco (2 mentions)
Microtof q 2 spectrometer, by Bruker (2 mentions)
Spd 20a, by Shimadzu (2 mentions)
62 protocols using inova 500 spectrometer
1
Purification and Characterization of Organic Compound
2
NMR Spectroscopy of Deuterated Compounds
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Samples were exchanged once with 99.9 atom% D2O with intermediate lyophilization, finally dissolved in 650 μL D2O. One- and two-dimensional 1H and 13C NMR spectra were recorded at a probe temperature of 25 °C on a Varian Inova 500 spectrometer (NMR Department, University of Groningen). Chemical shifts are expressed in parts per million in reference to external acetone (δ 1H 2.225; δ 13C 31.08). 1D 500-MHz 1H NMR spectra were recorded with 5000 Hz spectral width at 16k complex data points, using a WET1D pulse to suppress the HOD signal. Homonuclear decoupled 1D 125 MHz 13C NMR spectra were recorded with 31,000 Hz spectral width at 64k complex data points. 2D 1H-13C HSQC spectroscopy was performed using multiplicity editing, rendering CH2 signals in the negative plane, while CH and CH3 remain in the positive plain. 2D 13C-1H HMBC spectroscopy was performed suppressing single-bond correlations. Spectra were processed using MestReNova v9.1 (Mestrelabs Research SL, Santiago de Compostela, Spain).
3
Spectroscopic Characterization of Compounds
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NMR spectra were recorded using a Varian 500-MHz NMR spectrometer (Inova 500 Spectrometer, Varian, Palo Alto, CA, USA) with tetramethylsilane as an internal standard, and chemical shifts were recorded in ppm (δ). ESI-MS was conducted using an LCQ Fleet Ion Trap mass spectrometer (Thermo Scientific, Madison, WI, USA). Column chromatography (CC) was performed using silica gel (Kieselgel 60, 230–400 mesh; Merck) and Sephadex LH-20 (18–111 μm; GE Healthcare AB, Stockholm, Sweden). Thin-layer chromatography was performed using pre-coated silica Q-gel 60 F254 plates (0.25 mm; Merck), and preparative HPLC was carried out using the Varian Prostar 210 system with a YMC-Pack ODS-A column (5 μm, 250 × 20 mm i.d.; YMC, Kyoto, Japan). MPLC (IsoleraTM One) silica gel column chromatography was performed on Biotage® equipment with a Biotage® SNAP cartridge HP-SIL (25–100 g) silica gel column.
4
Chemical Reagents Procurement and NMR Analysis
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Example 29
All chemical reagents were obtained at 99% purity from Sigma-Aldrich, Alfa Aesar, or Mallinckrodt Chemicals. Magnesol® XL was purchased from The Dallas Group of America, Inc. 1H-NMR spectra were obtained using a Varian Inova 500 spectrometer (500 MHz); all spectra were recorded in CDCl3. Chemical shifts were reported in parts per million (ppm) and were referenced to residual protio-solvent resonances. Deuterated solvents used for 1H-NMR and SANS experiments (CDCl3 and d12-cyclohexane) were purchased from Cambridge Isotope Laboratories. Cylindrical quartz “banjo” cells used in scattering experiments were purchased from Hellma Analytics.
5
Analytical Techniques for Natural Product Isolation
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Thin-layer chromatography was carried out using pre-coated silica Q-gel 60 F254 plates (0.25 mm, Merck). Column chromatography (CC) was conducted using silica gel (Kieselgel 60, 230–400 mesh, Merck), and Sephadex LH-20 (18–111 µm, GE Healthcare AB, Stockholm, Sweden). HPLC was performed using the Varian Prostar 210 system. A YMC-Pack ODS-A column (5 μm, 250 × 20 mm i.d., YMC, Kyoto, Japan) was used for preparative HPLC analysis with an 8 mL/min flow rate. ESI-MS was performed on an LCQ Fleet Ion Trap mass spectrometer (Thermo Scientific, Madison, WI, USA). NMR spectral data were acquired by using a Varian 500-MHz NMR spectrometer (Inova 500 Spectrometer, Varian, Palo Alto, CA, USA). Tetramethylsilane was used as an internal standard, and chemical shifts data were expressed as δ value.
6
NMR and SEC Characterization of Polymers
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NMR spectroscopy was performed
on a 500 MHz Varian INOVA-500 spectrometer in DMSO-d6 with a d1 relaxation time of 10 s.
Size exclusion
chromatography (SEC) was used to determine molar masses and molar
mass distributions, using LS detectors. Full traces (Figure S1 ) were plotted from refractive index signals, relative
to polystyrene standards. PNiPAm and PDMAm samples were analyzed using
THF as the mobile phase, PHEAm samples were analyzed using dimethylformamide
as the mobile phase, and HPMC was analyzed using a mobile phase of
0.1 M Na2SO4 aqueous solution supplemented with
1% acetic acid. Molar mass data for HPMCAS were provided by The Dow
Chemical Company.
on a 500 MHz Varian INOVA-500 spectrometer in DMSO-d6 with a d1 relaxation time of 10 s.
Size exclusion
chromatography (SEC) was used to determine molar masses and molar
mass distributions, using LS detectors. Full traces (
to polystyrene standards. PNiPAm and PDMAm samples were analyzed using
THF as the mobile phase, PHEAm samples were analyzed using dimethylformamide
as the mobile phase, and HPMC was analyzed using a mobile phase of
0.1 M Na2SO4 aqueous solution supplemented with
1% acetic acid. Molar mass data for HPMCAS were provided by The Dow
Chemical Company.
7
Spectroscopic Analysis of Organic Compounds
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Melting points were determined on a Yanaco micro-melting point apparatus (Yanaco, Tokyo, Japan) and are uncorrected. Optical rotations were measured using a Jasco DIP-370 polarimeter (Jasco, Easton, MD, USA) in CHCl3. Ultraviolet (UV) spectra were obtained on a Jasco UV-240 spectrophotometer (Jasco, Easton, MD, USA). Infrared (IR) spectra (neat or KBr) were recorded on a Perkin Elmer 2000 FT-IR spectrometer (PerkinElmer, Waltham, MA, USA). Nuclear magnetic resonance (NMR) spectra, including correlation spectroscopy (COSY), nuclear Overhauser effect spectrometry (NOESY), rotating frame nuclear Overhauser effect spectrometry (ROESY), heteronuclear multiple-bond correlation (HMBC), and heteronuclear single-quantum coherence (HSQC) experiments, were acquired using a Varian Inova 500 spectrometer operating at 500 MHz (1H) and 125 MHz (13C), respectively, with chemical shifts given in ppm (δ) using tetramethylsilane (TMS) as an internal standard. Electrospray ionization (ESI) and high-resolution electrospray ionization (HRESI) mass spectra were recorded on a Bruker APEX II mass spectrometer (Bruker, Bremen, Germany). Silica gel (70–230, 230–400 mesh) (Merck, Darmstadt, Germany) was used for column chromatography (CC). Silica gel 60 F-254 (Merck, Darmstadt, Germany) was used for thin-layer chromatography (TLC) and preparative thin-layer chromatography (PTLC).
8
Characterization of Polymeric Nanoparticles
9
Spectroscopic Analysis of SP-IQ Coordination
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The reagents were purchased from Sigma-Aldrich (St. Louis, MO, USA). 1H- and 13C-NMR spectra were recorded in CDCl3 at 400 and 101 MHz, respectively, using an Inova 500 spectrometer (Varian, Palo Alto, CA, USA). UV-Vis absorption spectra were measured using a quartz cuvette in a UV-2401PC spectrophotometer (Shimadzu, Kyoto, Japan). Fluorescence spectra were measured on an AMINCO-Bowman Series 2 spectrofluorometer (Silver Spring, MD, USA). Unless otherwise noted, the concentration of SP-IQ is 1 × 10−5 M in CH3CN/H2O (1/1, v/v). For spectrophotometric titrations, the concentration of Co2+ and In3+ are used in the range of 0~45 μM and 0–100 μM, respectively.
10
NMR and Mass Spectrometry Analysis
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