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Arx 300

Manufactured by Bruker
Sourced in Switzerland, Germany, United States

The Bruker ARX-300 is a nuclear magnetic resonance (NMR) spectrometer designed for routine analysis and research applications. It operates at a magnetic field strength of 7.05 Tesla, providing a proton frequency of 300 MHz. The ARX-300 is capable of performing various NMR experiments to characterize the structure and properties of chemical compounds.

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29 protocols using arx 300

1

Characterization of Precursors 1 and 2

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Precursors 1 and 2 were obtained from commercial suppliers (TCI, Sigma Aldrich, St. Louis, MO, USA) and used as the samples. The 1H NMR spectrum was obtained with a Bruker (ARX 300, Billerica, MA, USA) using a Bruker (ARX 300). A Thermo FT-IR Nicolet iS 10 (Thermo Fisher, Waltham, MA, USA) was used to measure the FT-IR spectra in ATR in the range of 400–4000 cm−1. Mass spectroscopy samples were analyzed on a Thermo Scientific LCQ Fleet mass spectrometer.
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2

Purification and Characterization of Organic Compounds

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Purification of reaction products was carried out by column chromatography using silica gel (0.063–0.200 mm). Analytical thin-layer chromatography was performed on 0.25 mm silica gel 60-F plates. ESI ionization method and mass analyzer type MicroTof-Q were used for the HRMS measurements. NMR spectra were recorded at room temperature on a Bruker ARX300 or AV400 instruments. 1H-NMR spectra were recorded at 300 or 400 MHz, and 13C-APT-NMR spectra were recorded at 75 or 100 MHz, using DMSO-d6 as the deuterated solvent. Chemical shifts were reported in the δ scale relative to residual DMSO (2.50 ppm) for 1H-NMR and to the central line of DMSO-d6 (39.43 ppm) for 13C-APT-NMR. A Branson 5510 ultrasonic bath is used in the synthesis of the final compounds. Melting points were determined on a Gallenkamp variable heating apparatus. IR spectra were recorded on a PerkinElmer FT-IR 2,400 microanalyzer.
All commercially available solvents and reagents were used as received.
The Softwares used to perform the Figures are ChemBioDraw Ultra 9.0, Origin Pro 9.0 and Powerpoint 2010.
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3

Spectroscopic and Chromatographic Characterization

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The UV spectra were conducted on a UV-2201 spectrometer (Shimadzu, Kyoto, Japan). The FT-IR spectra were obtained on a Bruker IFS-55 spectrometer (Bruker, Ettlingen, Germany) by a KBr disk method. ESI-MS spectra were conducted on an Agilent 1100 ion trap spectrometer (Agilent Technologies, Palo Alto, CA, USA). HRESI-MS was recorded on a QFT-ESI mass spectrometer (Varian, Palo Alto, CA, USA). 1H-NMR and 13C-NMR spectra were recorded on Bruker ARX-300 and AV-600 NMR spectrometers (Bruker, Ettlingen, Germany) using pyridine-d5 as an internal standard [δH/C 7.20, 7.57, 8.72/123.44, 135.43, 149.84 (C5D5N)]. Optical rotations were measured with a Perkin-Elmer 241 polarimeter (Perkin-Elmer, Boston, MA, USA). The chromatographic silica gel (200−300 mesh) was purchased from Qingdao Ocean Chemical Factory (Qingdao, China) and ODS (50 μm) was purchased from YMC Co. Ltd, Kyoto, Japan. Sephadex LH-20 was purchased from GE Healthcare, Uppsala, Sweden. RP-HPLC analysis and semi-preparation were conducted using HITACHI L2130 series pumping system equipped with a HITACHI L2400 UV detector (Tokyo, Japan) and performed with a C-18 column (10 × 250 mm, 10 μm; YMC Co. Ltd, Kyoto, Japan).
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4

Analytical Characterization of Chemical Compounds

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NMR spectra were obtained at 300 or 500 (1H) and 75 or 125 (13C) MHz using Bruker ARX300 or Bruker DX-2 500 [QNP probe or multinuclear broadband observe (BBO) probe, respectively] spectrometers. Column chromatography was performed with 230–400 mesh silica gel. The melting points were determined using capillary tubes with a Mel-Temp apparatus and are uncorrected. IR spectra were obtained using a PerkinElmer 1600 series FTIR spectrometer on salt plates or as KBr pellets. ESIMS analyses were recorded on a FinniganMAT LCQ Classic mass spectrometer. APCI–MS analyses were performed using an Agilent 6320 ion trap mass spectrometer. EI/CIMS analyses were obtained with a Hewlett-Packard Engine mass spectrometer. All mass spectral analyses were performed at the Campus-Wide Mass Spectrometry Center of Purdue University. HPLC analyses were carried out on a Waters 1525 binary HPLC pump/Waters 2487 dual λ absorbance detector system using a 5 μm C18 reverse phase column. All reported yields refer to pure isolated compounds. Chemicals and solvents were of reagent grade and used as obtained from commercial sources without further purification. The purities of all of the biologically tested compounds were ≥95% as estimated by HPLC or determined by elemental analysis. For HPLC, the peak area of the major product was ≥95% of the combined total peak areas when monitored by a UV detector at 254 nm.
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5

Synthesis and Characterization of O-Acylterpineol Derivatives

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The chemical structures and reaction sequences of O-acylterpineol derivatives are listed in Supporting Information. The purity of each compound was over 98% as shown by gas chromatography (GC-14C, Shimadzu, Japan). The structures of the compounds were confirmed by NMR (ARX-300, Bruker, Switzerland) and HPLC-MS (ZQ-2000, Waters, USA). The 1HNMR and MS data are as follows:
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6

Synthesis and Characterization of Precursor 2

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Precursor 2 was synthesized according to our previously reported procedure [57 (link),58 (link)]. Unless otherwise noted, chemical reagents and solvents were purchased from commercial suppliers (Tokyo Chemical Industry (TCI), Sigma Aldrich) and used without further purification. Using a Bruker (ARX 300) and Bruker (DRX-500), the 1H and 13C NMR spectra of the samples were obtained. The optical absorption spectra of the samples were obtained at 298 K using a UV-vis spectrophotometer (Thermo Evolution 600). A Thermo FT-IR Nicolet iS 10 was used to measure the FT-IR spectra in ATR, in the range of 400–4000 cm−1. Mass spectroscopy sample were analyzed on a Thermo Scientific LCQ Fleet mass spectrometer. Powder XRD patterns were measured on a Bruker AXS D8 Advance A25.
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7

Synthesis and Characterization of Organic Compounds

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Unless otherwise noted, all the materials were obtained from commercially available sources and were used without purification. Thin-layer chromatography was performed on GF254 silica gel plates to monitor the reaction, and the plates were examined under UV light. The purification of the products was performed using column chromatography (60 Å, 200–300 mesh, Qingdao Ocean Chemicals or 120 Å, S-50mm, YMC Co., Ltd.), or silica gel plates (0.25 mm layer, Qingdao Ocean Chemicals) with the designated solvents. IR spectra were obtained using a JASCO FT/IR-480 plus spectrometer. 1H and 13C NMR spectra were taken in CDCl3 solution on Bruker ARX-300 and Bruker AV-600 spectrometers with TMS as the internal reference. Chemical shifts were reported in ppm downfield from tetramethylsilane and proton–proton coupling constants (J) in Hz. ESI-MS spectrawere performed on a Finigan LCQ Advantage MAX mass spectrometer.
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8

Nuclear Magnetic Resonance Spectroscopy Protocol

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1H and 13C nuclear magnetic resonance (NMR) spectra
were recorded on Varian Gemini 300, Varian Mercury 300, Bruker ARX
300, Bruker DRX 400, Bruker AV 400, and Bruker AV-NEO 500 spectrometers
at 300, 400, or 500 MHz (1H) and 75 MHz, 100 MHz, or 125
MHz (13C), respectively. Chemical shifts (δ) are
reported in parts per million downfield from tetramethylsilane using
the residual deuterated solvent signals as an internal reference.
For 1H NMR, coupling constants J are given
in hertz, and the resonance multiplicity is described as s (singlet),
d (doublet), t (triplet), q (quartet), m (multiplet), and br (broad).
All spectra were recorded at 25 °C. Mass spectrometry (MS) and
high-resolution mass spectrometry (HR-MS) were performed by the MS-service
of the Laboratory for Organic Chemistry at the ETH Zürich on
a Waters Micromass AutoSpec-Ultima spectrometer (EI), on a Bruker
maXis spectrometer (ESI), or on a Varian IonSpec FT-ICR spectrometer
(MALDI). For MALDI measurements, the matrix was 2-[(2E)-3-(4-tert-butylphenyl)-2-methylprop-2-enylidene]malononitrile
(DCTB) or 3-hydroxypyridine-2-carboxylic acid (3-HPA). Masses are
reported in m/z units for the molecular
ion M+ for the exact
(ChemDraw) and the detected mass. NMR spectra can be obtained upon
request.
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9

Cytotoxicity Evaluation of PEGylated Nanoparticles

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All chemicals were procured
from Sigma-Aldrich Chemical Company, J&K Chemical Company or AMRESCO
and used as received. All organic solvents were purchased from Beijing
Chemical Works and used without further purification. NH2-PEG10-COOH were purchased from Yanyi Biotech Company
Shanghai. Dulbecco’s modified Eagle’s medium (DMEM)
was purchased from HyClone/Thermo Fisher (Beijing, China). (3-(4,5′-Dimethylthiazol-2′yl)-2,5-dipehenyl-2H-tetrazolium hydrobromide) (MTT) was purchased from Xinjingke
Biotech (Beijing, China) and dissolved in 1× phosphate-buffered
saline (PBS) before use. The 1H NMR and 13C
NMR spectra were recorded on Bruker ARX 300 and ARX 400 instruments
with tetramethylsilane as the internal standard. High-resolution mass
spectra (HRMS) were taken on a Bruker 9.4T Solarix FT-ICR-MS spectrometer.
The UV–vis absorption spectrum was measured on a JASCO V-550
spectrophotometer. The fluorescence spectrum was taken on a Hitachi
F-4500 fluorometer equipped with a Xenon lamp excitation source. Absolute
fluorescence quantum yield was measured on Hamamatsu absolute photoluminescence
quantum yield spectrometer C11347. The MTT assay was performed on
a BIO-TEK Synergy HT microplate reader. Cell counting was performed
on an automated cell counter (Countess, Invitrogen). Cell imaging
was recorded by a confocal laser scanning microscope (FV 1000-IX81,
Olympus, Japan).
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10

Synthesis and Characterization of Organometallic Compounds

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All reactions were carried out under a dry nitrogen atmosphere by using Schlenk techniques. Organic solvents were dried and distilled under nitrogen and degassed prior to use. Unless otherwise stated, reagents were obtained from commercial sources and used as received. 1H- and 13C-NMR spectra were recorded on a Bruker ARX 300 (300.1 MHz for 1H, 75.5 MHz for 13C) using D2O or CDCl3 as solvents. 1H- and 13C-NMR spectra for each compound are shown in S1 Appendix. C, H, and N analyses were performed by The Analytical Services of the Universidad Nacional del Sur (Argentina) with an Exeter Analytical Inc. CE-440 microanalyzer.
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