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5 protocols using unity 500 mhz

1

Synthesis and Characterization of Poly(Succinimide) Derivatives

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PSI was synthesized
by acid-catalyzed
polycondensation of l-aspartic acid (Sigma, MO).1 (link) Designated amounts of 2-AEMA (Sigma) and ethanolamine
were added sequentially to PSI dissolved in dimethylformamide. The
molar ratio of 2-AEMA was adjusted to regulate the DS of MA groups
(DSMA) from 0 to 10%. The molar ratio of ethanolamine was
adjusted to regulate the DS of hydroxyl groups from 95 to 85%, respectively.
The molar amounts of the reagents used for the reactions are listed in Table 2.
The
resulting polymer was dissolved in DMSO-d6 (Cambridge Isotope Laboratories, Inc.) and analyzed by 1H NMR (Varian Unity 500 MHz). DSMA and DSOH were calculated from the integrated peaks of the 1H NMR
spectra using the following equations2 (link)
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2

Comprehensive NMR and Mass Spectrometry Analysis

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NMR spectra were collected on a Varian Unity 500 MHz (500 MHz and 125 MHz for the 1H and 13C nuclei respectively), a Varian VX 500 MHz with 13C-optimized cryoprobe, and a Bruker 600 MHz (600 MHz and 150 MHz for the 1H and 13C nuclei respectively) with 1.7 mm inverse cryo-probe. NMR experiments were conducted using CDCl3 from Cambridge Isotope Laboratories, Inc. 99.8% D, containing 0.03% or 1.0% v/v trimethylsilane (referencing δH 0.0 as the internal standard from trimethylsilane, and δC 0.0 or δC 77.16 as internal standards using trimethylsilane and CDCl3, respectively). Microwave-heated reactions were run in a Biotage Initiator microwave synthesizer. LR-LCMS data were collected on a Thermo Finnigan Surveyor Autosampler/LC-Pump-Plus/PDA-Puls with a Thermo Finnigan Advantage Max mass spectrometer. HRMS data was collected on a Finnigan LTQ-FTICR-MS instrument (Thermo-Electron Corporation, San Jose, CA) fitted with either an Ion-Max ESI source for LCMS runs, or a Biversa Nanomate (Advion Biosystems, Ithaca, NY) electrospray source. HPLC purification was carried out with a Waters 515 HPLC Pump with a Waters 996 Photodiode Array Detector using Empower Pro software. All solvents were HPLC grade except for H2O which was purified with a Millipore Milli-Q system before use, CH3CN which was LCMS grade from J.T. Baker, and acetone which was distilled before use.
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3

NMR and Mass Spectrometry Analysis

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1H NMR spectra were acquired using Varian Unity 500 MHz (13C, 126 MHz) spectrometer. 1H NMR chemical shifts (δ) are reported in parts per million (ppm) and were referenced to the residual solvent peak at 7.26 ppm for CDCl3 and 2.50 ppm for DMSO-d6. 13C NMR chemical shifts are reported in ppm and were referenced to the residual solvent peak at 77.16 ppm for CDCl3 and 39.52 ppm for DMSO-d6. All NMR spectra were original one which was scanned. Mass spectra were obtained on Micromass Q-Tof Ultima (HR-ESI) and Micromass Quattro (LR-ESI) instruments. MALDI-TOF-MS was carried out using Applied Biosystems Voyager-DE STR with a nitrogen laser (337 nm, 3 ns pulse, 20 Hz maximum firing rate) and using 2-(4′-hydroxybenzeneazo)benzoic acid (HABA) as matrix.
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4

Comprehensive Spectroscopic Analysis of Compounds

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NMR spectra (1H, 13C, COSY, HSQC, HMBC and NOESY) were measured on a Varian Unity 500 MHz (Varian Inc., Palo Alto, CA, USA) and a Bruker 600 MHz (Bruker BioSpin GmbH, Rheinstetten, Germany) spectrometer with TMS as an internal standard. Optical rotations were obtained on a Rudolph Research Analytical Autopol III polarimeter (Rudolph Research Analytical, Hackettstown, NJ, USA). CD spectra were recorded on a JASCO J-1500 spectrometer (JASCO Corporation, Tokyo, Japan). UV spectra were acquired on a Shimadzu UV-1650PC spectrophotometer (Shimadzu Corporation, Kyoto, Japan). IR spectra were measured on a JASCO FT/IR-4100 spectrophotometer (JASCO Corporation, Tokyo, Japan). HRESIMS were measured on Waters Synapt HDMS LC/MS mass spectrometer (Waters Corporation, Milford, MA, USA). HPLC system was composed of a PrimeLine Binary pump (Analytical Scientific Instruments, Inc., El Sobrante, CA, USA) with RI-101 (Shoko Scientific Co. Ltd., Yokohama, Japan), semi-preparative ODS column (YMC-Pack-ODS-A, 250 × 10 mm i.d, 5 µm) and an analytical ODS column (YMC-Pack-ODS-A, 250 × 4.6 mm i.d, 5 µm)(YMC Corporation, Kyoto, Japan).
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5

Synthesis and Characterization of Organic Compounds

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1, 4-dioxane aqueous, kieselguhr, anhydrous ethanol, anhydrous acetonitrile, sodium carbonate, acetone, sodium hydroxide, and hydrochloric acid were purchased from SCRC. Bathocuproine (BC), selenium dioxide, sodium borohydride, and hydrobromic acid was purchased from ABCR. Diethyl iminodiacetat was purchased from Sigma. Anhydrous ethanol was distilled from magnesium and iodine. Anhydrous acetonitrile was distilled from phosphorus pentoxide.
1H NMR spectra were recorded on Varian Unity+ 500M Hz. 1H NMR spectra were registered in D2O, and chemical shifts are expressed in partsper million (δ) relative to internal Me4Si. IR spectra were recorded on a Nicolet Avatar 330 FTIR spectrophotometer. Mass spectra were recorded by Bruke BioTOF-Q. UV spectra were recorded on a Persee TU-1900 ultraviolet and visible spectrophotometer.
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