All the chemicals and reagents were purchased from commercial suppliers (Sigma-Aldrich, Alfa Aesar, ACS Scientific, Acros, Ambeed, Combi-blocks) and used without any further purification. All dry reactions were carried out under argon in flame-dried glassware with magnetic stirring using standard gas-tight syringes, cannula, and septa. 1H and 13C NMR spectra were measured on Bruker DPX-500 (operating at 500 MHz for 1H and 125 MHz for 13C) or Bruker DPX-400 (operating at 400 MHz for 1H and 100 MHz for 13C), 19F was measured on Bruker DPX-400 (operating at 375 MHz). Tetramethylsilane (TMS) (0 ppm) and/or CDCl3 (7.26 ppm) served as the internal standard for 1HNMR, CDCl3 was used as the internal standard (77.0 ppm) for 13CNMR, and trifluorotoluene served as the internal standard (−63 ppm) for 19F NMR. HRMS analyses were performed using a Q Exactive Plus Mass Spectrometer at the Proteomics Facility of the University of Rochester. Silica gel chromatography purifications were carried out using AMD Silica Gel 60 230-400 mesh. Thin Layer Chromatography (TLC) was carried out using Merck Millipore TLC silica gel 60 F254 glass plates.
Dpx 400
Manufactured by Bruker
Sourced in Germany, United States, Switzerland
The DPX-400 is a versatile nuclear magnetic resonance (NMR) spectrometer designed for a range of analytical applications. It operates at a frequency of 400 MHz and is capable of performing various NMR experiments to analyze the structure and properties of chemical compounds.
Automatically generated - may contain errors
Lab products found in correlation
Dpx 300, by Bruker (10 mentions)
Dpx 500, by Bruker (7 mentions)
Avance 400, by Bruker (7 mentions)
Av 400, by Bruker (6 mentions)
Tlc silica gel 60 f254 glass plates, by Merck Group (5 mentions)
Vector 22 ftir spectrometer, by Bruker (3 mentions)
Lc it tof ms, by Shimadzu (3 mentions)
Escalab 250, by Thermo Fisher Scientific (3 mentions)
Spd 20a vp detector, by Shimadzu (2 mentions)
Lc ms msd, by Hewlett-Packard (2 mentions)
Aviii400, by Bruker (2 mentions)
Aviii 500, by Bruker (2 mentions)
Drx 500, by Bruker (2 mentions)
3100 ft ir spectrometer, by Agilent Technologies (2 mentions)
Diamond attenuated total reflection cell, by Bruker (2 mentions)
Synergy multidetection microplate reader, by Agilent Technologies (2 mentions)
Pl as rt mt auto, by Agilent Technologies (2 mentions)
390 lc mds system, by Agilent Technologies (2 mentions)
Fourier transform ir 6300 ft ir spectrometer, by Jasco (2 mentions)
D max rapid 2, by Bruker (2 mentions)
93 protocols using dpx 400
1
Optimized Organic Synthesis Procedures
2
Characterization of Organic Compounds
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All the chemicals and reagents
were purchased from commercial suppliers (Sigma-Aldrich, Alfa Aesar,
ACS Scientific, Acros, Ambeed, Combi-blocks) and used without any
further purification. All dry reactions were carried out under argon
in flame-dried glassware with magnetic stirring using standard gastight
syringes, cannula, and septa. 1H and 13C NMR
spectra were measured on Bruker DPX-500 (operating at 500 MHz for 1H and 125 MHz for 13C) or Bruker DPX-400 (operating
at 400 MHz for 1H and 100 MHz for 13C), and 19F was measured on Bruker DPX-400 (operating at 375 MHz).
Tetramethylsilane (TMS) (0 ppm) and/or CDCl3 (7.26 ppm)
served as the internal standard for 1H NMR, CDCl3 was used as the internal standard (77.0 ppm) for 13C
NMR, and trifluorotoluene served as the internal standard (−63
ppm) for 19F NMR. HRMS analyses were performed using a
Q Exactive Plus mass spectrometer at the Proteomics Facility of the
University of Rochester. Silica gel chromatography purifications were
carried out using AMD silica gel 60 230–400 mesh. Thin layer
chromatography (TLC) was carried out using Merck Millipore TLC silica
gel 60 F254 glass plates.
were purchased from commercial suppliers (Sigma-Aldrich, Alfa Aesar,
ACS Scientific, Acros, Ambeed, Combi-blocks) and used without any
further purification. All dry reactions were carried out under argon
in flame-dried glassware with magnetic stirring using standard gastight
syringes, cannula, and septa. 1H and 13C NMR
spectra were measured on Bruker DPX-500 (operating at 500 MHz for 1H and 125 MHz for 13C) or Bruker DPX-400 (operating
at 400 MHz for 1H and 100 MHz for 13C), and 19F was measured on Bruker DPX-400 (operating at 375 MHz).
Tetramethylsilane (TMS) (0 ppm) and/or CDCl3 (7.26 ppm)
served as the internal standard for 1H NMR, CDCl3 was used as the internal standard (77.0 ppm) for 13C
NMR, and trifluorotoluene served as the internal standard (−63
ppm) for 19F NMR. HRMS analyses were performed using a
Q Exactive Plus mass spectrometer at the Proteomics Facility of the
University of Rochester. Silica gel chromatography purifications were
carried out using AMD silica gel 60 230–400 mesh. Thin layer
chromatography (TLC) was carried out using Merck Millipore TLC silica
gel 60 F254 glass plates.
3
Characterization of New Organic Compounds
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FT-IR spectra were recorded on a Mattson-Galaxy Satellite FT-IR spectrophotometer containing a MKII Golden Gate Single Reflection ATR System. Elemental analyses were performed using a CHNS-O Elemental Analyser EA-1108 from Fisons. UV-Vis spectroscopy was performed on a Cary 50 Scan (Varian) UV-Vis spectrophotometer with 1 cm quartz cells or with an immersion probe of 5 mm path length. NMR spectra have been recorded with a Bruker ARX 300 or a DPX 400 instrument equipped with the appropriate decoupling accessories. -2013 (Sheldrick, 2013). For structure 3, two disordered ethyl ether solvent molecules per asymmetric unit were removed using the SQUEEZE option in PLATON. 34 The crystallographic data as well as details of the structure solution and refinement procedures are reported in Table 1. CCDC 1471844 (1) and 1471845 (3) contain the supplementary crystallographic data for this paper.
4
Quantifying CD and Linalool Interactions
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HPbCD/linalool-IC-NF, MbCD/linalool-IC-NF, and HPcCD/ linalool-IC-NF (all 10 mg) were dissolved in 500 mL of d6-DMSO to calculate the molar ratio of each CD and linalool. Then, proton nuclear magnetic resonance ( 1 H NMR) spectra were recorded for each solution using a Bruker DPX-400. The integration of the chemical shifts (d) was calculated via Mestrenova software. In addition, 1 H NMR spectra were recorded for nanofibers (10 mg) after incubating them at RT for 25 days.
5
Andrographolide Derivative Synthesis and Characterization
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The reaction
progress and purity of the andrographolide (1 ) and its
derivatives were checked by thin-layer chromatography using Merck
precoated silica gel 60 F254 plates. TLC visualization was attained
under UV light at 254 nm or exposure to iodine vapors. A Buchi Rotavapor
was used for concentration of organic solvents. Column chromatography
using silica gels (60–120, 100–200 mesh) was performed
for purification of synthesized compounds. NMR spectra (1H and 13C) were recorded on Bruker DPX 400 and DPX 500
using CDCl3, CD3OD, D2O, and DMSO-d6 as solvent and TMS as an internal standard. The chemical
shifts (δ) are expressed in parts per million (ppm) referenced
to the residual solvent, and the coupling constant (J value) is given in hertz (Hz). The MestReNova software was used
for processing of NMR spectra, and signal multiplicity is expressed
as follows: s (singlet), br s (broad singlet), d (doublet), t (triplet),
q (quartet), and m (multiplet). HRMS (high-resolution mass spectra)
were taken from an Agilent Technology instrument (6540). Unless indicated,
all the reagents and solvents used for synthesis and purification
were purchased from Sigma-Aldrich/Merck and used as such without further
purification.
progress and purity of the andrographolide (
derivatives were checked by thin-layer chromatography using Merck
precoated silica gel 60 F254 plates. TLC visualization was attained
under UV light at 254 nm or exposure to iodine vapors. A Buchi Rotavapor
was used for concentration of organic solvents. Column chromatography
using silica gels (60–120, 100–200 mesh) was performed
for purification of synthesized compounds. NMR spectra (1H and 13C) were recorded on Bruker DPX 400 and DPX 500
using CDCl3, CD3OD, D2O, and DMSO-d6 as solvent and TMS as an internal standard. The chemical
shifts (δ) are expressed in parts per million (ppm) referenced
to the residual solvent, and the coupling constant (J value) is given in hertz (Hz). The MestReNova software was used
for processing of NMR spectra, and signal multiplicity is expressed
as follows: s (singlet), br s (broad singlet), d (doublet), t (triplet),
q (quartet), and m (multiplet). HRMS (high-resolution mass spectra)
were taken from an Agilent Technology instrument (6540). Unless indicated,
all the reagents and solvents used for synthesis and purification
were purchased from Sigma-Aldrich/Merck and used as such without further
purification.
6
Characterization of Organic Compounds
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Chemicals, reagents and analytical grade solvents were purchased from Sigma-Aldrich (Gillingham, UK) unless specified. All reactions were carried out under argon. 1H and 13C NMR spectra were recorded in deuterated dimethyl sulfoxide (DMSO-d6) using a Bruker DPX 400 (400 MHz) spectrometer where chemical shifts (δ) were reported as parts per million (ppm) relative to tetramethylsilane (TMS) as internal standard. Coupling constants (J) are reported in Hertz (Hz) and multiplicities are reported as follows: s (singlet), d (doublet), t (triplet), or m (multiplet). Infrared spectra were recorded on a Perkin Elmer precisely spectrum 100 FT-IR spectrometer. Mass spectrometry data were recorded on a Thermo Fisher LTQ Orbitrap XL instrument. CHN elemental analyses for metal compounds were obtained from MEDAC LTD (Woking, UK), analytical and consultancy services.
7
Characterization of Ga(III) Complexes
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Reactions were performed in standard lab glassware when appropriate. Water was freshly distilled before use. All other solvents used were of HPLC grade quality. ESI mass spectrometry was performed by using a Waters (Manchester, UK) ZMD mass spectrometer equipped with a single quadrupole analyser. Samples were introduced to the mass spectrometer by flow injection using a Waters 600 pump (flow rate 0.1 mL min−1 MeCN) and Waters 2700 autosampler. 1H and 19F{1H} NMR spectra were recorded in solution in deuterated H2O or methanol on a Bruker DPX-400 or AV-400 spectrometers and are referenced to the residual solvent protons (1H) and CCl3F (19F) at 298 K. IR spectra were recorded neat (oils) or as Nujol mulls (solids) between CsI plates by using a Perkin–Elmer Spectrum 100 spectrometer over the range 4000–200 cm−1. Microanalyses were undertaken by Stephen Boyer at London Metropolitan University. Compounds Bz(CH2CO2H)2-tacn⋅HCl (H2L⋅HCl)[5a ] and Li2[Bz(CH2CO2)2-tacn] (Li2L)[9 ] were prepared by using the literature methods; Ga(NO3)3⋅9 H2O and GaF3⋅3 H2O were obtained from Aldrich and used as received.
8
NMR and HPLC Characterization of Compounds
9
Synthesis and Characterization of Novel Compounds
10
Organic Compound Characterization Methods
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All chemicals were reagent grade and used without further purification. Column chromatography was performed with Kanto Chemical silica gel 60 N (spherical, neutral). 1H NMR spectra were recorded on a Bruker AVANCE600 spectrometer (600 MHz), a Bruker DPX400 (400 MHz), or a Bruker AVANCE400 spectrometer (400 MHz). In NMR measurements, tetramethylsilane was used as an internal standard (0 ppm). CD spectra were recorded on a JASCO J-820 spectropolarimeter at 295 K. Mass spectra (ESI-TOF, positive mode) were recorded on an Applied Biosystems QStar Pulsar i spectrometer.
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