Infrared spectra were recorded as KBr pellets on a Perkin-Elmer Spectrum 100S (4000–250 cm−1 range) Fourier-Transform spectrometer. 1H NMR spectra (400 MHz) were recorded on a Bruker DPX-400 spectrometer with chemical shifts (δ) in ppm to high frequency of Si(CH3)4 and coupling constants (J) in Hz. 31P{1H} NMR (162 MHz) spectra were recorded on a Bruker DPX-400 spectrometer with chemical shifts (δ) in ppm to high frequency of 85% H3PO4. NMR spectra were measured in CDCl3 or (CD3)2SO at 298 K. Elemental analyses (Perkin-Elmer 2400 CHN Elemental Analyser) were performed by the Loughborough University Analytical Service within the Department of Chemistry.
Dpx 400 spectrometer
Manufactured by Bruker
Sourced in United States, Germany, Switzerland
The DPX-400 spectrometer is a nuclear magnetic resonance (NMR) instrument designed for high-resolution analysis of chemical samples. It operates at a frequency of 400 MHz and is capable of performing a range of NMR experiments to investigate the structure and properties of organic and inorganic compounds.
Automatically generated - may contain errors
Lab products found in correlation
Ir prestige 21, by Shimadzu (4 mentions)
Silica gel 60, by Merck Group (4 mentions)
Gcms qp5050a, by Shimadzu (3 mentions)
Biflex 3, by Bruker (2 mentions)
Exactive bench top lc ms spectrometer, by Thermo Fisher Scientific (2 mentions)
Q exactive, by Thermo Fisher Scientific (2 mentions)
Rf 540 fluorescence spectrophotometer, by Agilent Technologies (2 mentions)
8453 spectrophotometer, by Agilent Technologies (2 mentions)
Vertex 70 spectrophotometer, by Bruker (2 mentions)
R 100, by Büchi (2 mentions)
Lcms it tof mass spectrometer, by Shimadzu (2 mentions)
Alpha platinum atr fourier transform spectrometer, by Bruker (2 mentions)
Gctof hrms, by Waters Corporation (2 mentions)
Vertex 70 spectrometer, by Bruker (2 mentions)
Silica gel 60 f254, by Merck Group (2 mentions)
Uflc system, by Shimadzu (2 mentions)
Silica gel 60h, by Merck Group (2 mentions)
Milli q plus filter system, by Merck Group (2 mentions)
Topspin 4, by Bruker (2 mentions)
Kieselgel 60, by Merck Group (1 mentions)
96 protocols using dpx 400 spectrometer
1
Spectroscopic Characterization of Compounds
2
Synthesis and Characterization of Dysprosium Phthalocyanine Complexes
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1,2,4-Trichlorobenzene (TCB) and dichloromethane were freshly distilled from CaH2 under nitrogen. Column chromatography was carried out on silica gel columns (Merck, Kieselgel 60, 70–230 mesh) with the indicated eluents. All other reagents and solvents were used as received. The compounds of {(Pc)Dy[Pc(OC5H11)8]} and {[Pc(OC5H11)8]Dy[Pc(OC5H11)8]} were prepared according to the published procedure.
1H NMR spectra were recorded on a Bruker DPX 400 spectrometer in CDCl3. Spectrum was referenced internally using the residual solvent resonances (δ = 7.26 for 1H NMR). MALDI-TOF mass spectra were taken on a Bruker BIFLEX III ultrahighresolution Fourier transform ion cyclotron resonance (FT-ICR) mass spectrometer with alpha-cyano-4-hydroxycinnamic acid as matrix. Elemental analyses were performed on an Elementar Vavio El III.
1H NMR spectra were recorded on a Bruker DPX 400 spectrometer in CDCl3. Spectrum was referenced internally using the residual solvent resonances (δ = 7.26 for 1H NMR). MALDI-TOF mass spectra were taken on a Bruker BIFLEX III ultrahighresolution Fourier transform ion cyclotron resonance (FT-ICR) mass spectrometer with alpha-cyano-4-hydroxycinnamic acid as matrix. Elemental analyses were performed on an Elementar Vavio El III.
3
Characterization of Organic Compounds
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Melting points were determined using a MQAPF-307 melting point apparatus (Microquimica, Brazil) and remained uncorrected. The progress of the reactions was monitored by thin layer chromatography (TLC) in silica gel plates. Column chromatography was performed over silica gel (60–230 mesh). Infrared spectra were recorded on a Spectra One Perkin-Elmer spectrophotometer, fitted with a Paragon ATR accessory. Mass spectra (HRMS) were recorded on a Shimadzu GC MS-QP5050A instrument using direct insertion together with the electrospray ionization method and a quadrupole analyzer. The 1H, 13C, and DEPT 135 nuclear magnetic resonance (NMR) spectra and two dimensional NMR spectra—correlations spectroscopy (COSY), heteronuclear single-quantum correlation (HSQC), and heteronuclear multiple bound correlation (HMBC)—were recorded on a Bruker Avance DPX 200 and a DPX 400 spectrometer at 200 and 400 MHz using CDCl3 and DMSOd6 as the solvent and Tetramethylsylane (TMS) as the internal standard, unless otherwise stated. The NMR data are presented as follows: chemical shift in ppm, multiplicity, number of protons, J in Hz, and proton assignments. Multiplicities are indicated by the following abbreviations: s (singlet), d (doublet), dd (double doublet), t (triplet), q (quartet), m (multiplet), qn (quintet), st (sextet), ht (heptet), and bs (broad singlet).
4
NMR Spectroscopic Analysis of Samples
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NMR spectra were obtained on a Bruker DPX 400 spectrometer (400 MHz for 1H and 100 MHz for 13C). Samples were dissolved in CDCl3, and the spectra were calibrated using TMS signals. The chemical shifts are given in ppm. The carbon atoms in the alkyl chains of the acyloxy groups were numbered by labelling the carbon atom of the carbonyl group as number one and subsequently increasing towards the methyl terminus of the acyl chain. All 1H-NMR spectra were been added in Supplementary Materials .
5
Characterization of Organic Compounds
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Before using, all solvents were distilled, and experimental conditions for analytical TLC and column chromatography purification was used according to previous work. The electrothermal 9100 apparatus was used to determining melting points, and they are uncorrected. Microanalyses were performed on a Fisons EA 1108 CHNS-O instrument and were within ±0.4% of the calculated compositions. Bruker DPX-400 spectrometer was used to record NMR spectra. The assignment of chemical shifts is based on standard NMR experiments (1H, 13C, 1H-COSY, HSQC, HMBC, and NOE). The chemical shift values are expressed in ppm relative to tetramethylsilane as an internal standard. Shimadzu DI-2010 was used to determine the mass spectra.
6
Characterization of Molecular Assemblies
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NMR spectra were measured with a Bruker DPX-400 spectrometer. ESI mass spectra were obtained on Thermo Scientific™ Exactive™ Bench-Top LC-MS Spectrometer and Thermo Scientific™ Exactive™ Plus Bench-Top LC-MS Spectrometer. FT-IR spectroscopy was carried out with a Nicolet 6700 FT-IR spectrometer. Molecular assembly formation in solutions was analyzed by dynamic light scattering (DLS) by using Photal DLS-8000. UV and CD spectra were obtained on a Shimadzu UV-2450 spectrophotometer and a JASCO J600 circular dichroism spectrometer, respectively. The UV and CD spectra were obtained using a quartz optical cell with 1 cm path length at a concentration of 0.05 mM.
7
Characterization of Organic Compounds
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1H NMR spectra were recorded on a Bruker DPX 400 spectrometer in CDCl3. Spectrum was referenced internally using the residual solvent resonances (δ = 7.26 for 1H NMR). Electronic absorption spectra were recorded on a Hitachi U-4100 spectrophotometer. MALDI-TOF mass spectra were taken on a Bruker BIFLEX III ultra high resolution Fourier transform ion cyclotron resonance (FT-ICR) mass spectrometer with alpha-cyano-4-hydroxycinnamic acid as matrix. Elemental analysis was performed on an Elementar Vario El III. The open aperture Z-scan measurements and optical limiting property were carried out using a nanosecond laser at 532 nm.
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1H NMR spectra were recorded on a Bruker DPX 400 spectrometer in CDCl3. Spectrum was referenced internally using the residual solvent resonances (δ = 7.26 for 1H NMR). Electronic absorption spectra were recorded on a Hitachi U-4100 spectrophotometer. MALDI-TOF mass spectra were taken on a Bruker BIFLEX III ultra high resolution Fourier transform ion cyclotron resonance (FT-ICR) mass spectrometer with alpha-cyano-4-hydroxycinnamic acid as matrix. Elemental analysis was performed on an Elementar Vario El III. The open aperture Z-scan measurements and optical limiting property were carried out using a nanosecond laser at 532 nm.
8
Novel Synthetic Approach for Chiral Compounds
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All solvents and chemical reagents were purchased from Aladdin Reagent (Shanghai, China) and Energy Chemical (Shanghai, China), respectively. The melting points of all novel compounds were determined on an X-4B microscope melting point apparatus and were uncorrected (Shanghai Electrophysics Optical Instrument Co., LTD, Shanghai, China). Reactions were detected by thin-layer chromatography (TLC) and visualized under UV light at 254 nm. All 1H NMR and 13C NMR spectra data were recorded on a Bruker DPX-500 or a DPX-400 spectrometer (Bruker, Billerica, MA, USA), DMSO-d6 or CDCl3 were used as solvents, and tetramethylsilane was used as an internal standard. The high-resolution mass spectrometer (HRMS) data of the compounds were obtained using a Thermo Scientific Q-Exactive (Thermo Scientific, Missouri, MO, USA). The purity of that compounds was detected by HPLC, which was performed on a Shimadzu LC-2030 Plus (Shimadzu, Tokyo, Japan) with a Daicel Chiralpak AD-H column (conditions: 10% Isopropyl alcohol/Hexanes, 1.0 mL/min, λ = 220 nm, 30 °C). Chromatography was conducted on silica gel 200–300 mesh (Fluka, Daicel (China) investment Co., LTD, Shanghai, China) and under low pressure. The general experimental procedures that were used for the synthesis of all of the compounds is described in the following paragraphs.
9
Characterization of Naphthalyl-Amino Acid Complexes
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3-(2-naphthyl)-D-alanine and 3-(2-naphthyl)-L-alanine were obtained from Aldrich and used as supplied without further purification. Q[8] was prepared according to a literature method39 (link)40 . All the 1H NMR spectra were recorded on a Bruker DPX 400 spectrometer in D2O. Absorption spectra of the host-guest complexes were recorded on an Aglient 8453 spectrophotometer at room temperature. Fluorescence spectra of the host-guest complexes were performed with a Varian RF-540 fluorescence spectrophotometer. MALDI-TOF mass spectrometry was recorded on a Bruker BIFLEX III ultra-high resolution Fourier transform ion cyclotron resonance (FT-ICR) mass spectrometer with a-cyano-4-hydroxycinnamic acid as matrix.
10
NMR Spectroscopy of Compounds
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NMR spectra were captured on a BRUKER DPX-400 spectrometer (Billerica, MA, USA) at 400 and 100 MHz for 1H and 13C NMR, respectively. DMSO-d6 was used as a solvent.
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