IR spectra were recorded as Nujol mulls or neat thin films between CsI plates using a PerkinElmer Spectrum 100 instrument over the range 4000-200 cm -1 . 1 H and 13 C{ 1 H} NMR spectra were recorded from solutions in CDCl 3 or CD 2 Cl 2 on a Bruker AV400 spectrometer and referenced to TMS via the residual protio-solvent resonance. 125 Te{ 1 H} NMR spectra were recorded from solutions in CD 2 Cl 2 on a Bruker AV400 spectrometer and referenced to external neat TeMe 2 . Microanalytical results were obtained from Medac Ltd.
Av 400 spectrometer
Manufactured by Bruker
Sourced in United States, Germany, Switzerland, China
The AV-400 spectrometer is a nuclear magnetic resonance (NMR) instrument manufactured by Bruker. It operates at a frequency of 400 MHz and is designed for conducting high-resolution NMR analyses. The AV-400 spectrometer provides accurate and reliable data for a range of applications.
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Lab products found in correlation
Av 500 spectrometer, by Bruker (10 mentions)
Q star elite esi lc ms ms mass spectrometer, by Thermo Fisher Scientific (9 mentions)
Silica gel gf254 for tlc, by Merck Group (8 mentions)
Nicolet 6700, by Thermo Fisher Scientific (6 mentions)
Av 300, by Bruker (5 mentions)
Av 600 spectrometer, by Bruker (5 mentions)
V 550 uv vis spectrophotometer, by Jasco (4 mentions)
Agilent 6520 q tof, by Agilent Technologies (4 mentions)
Methanol, by Sinopharm (4 mentions)
Silica gel, by Qingdao Haiyang Chemical (4 mentions)
6210 esi tof mass spectrometer, by Agilent Technologies (3 mentions)
Ls55 spectrofluorometer, by PerkinElmer (3 mentions)
P 1020 polarimeter, by Jasco (3 mentions)
Facscalibur flow cytometer, by BD (3 mentions)
Uv 2600, by Shimadzu (3 mentions)
Vario micro cube chn analyzer, by Elementar (3 mentions)
Silica gel, by Qingdao Marine Chemical (3 mentions)
Lc ms 2010a, by Shimadzu (3 mentions)
Spectrum 100 spectrometer, by PerkinElmer (3 mentions)
Diamonsil c18, by Dikma Technologies (3 mentions)
267 protocols using av 400 spectrometer
1
Spectroscopic Characterization of Compounds
2
Synthetic Methodology for Novel Compounds
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Unless otherwise noted, materials were obtained commercially and used without further purification. All the solvents were treated according to general methods. Flash column chromatography was performed over silica gel (300 to 400 mesh). See Supplementary Materials and Methods for experimental details.
1H nuclear magnetic resonance (NMR) spectra were recorded on a Bruker AV-400 spectrometer and a Bruker AV-500 spectrometer in chloroform-d3. Chemical shifts are reported in parts per million (ppm) with the internal tet-ramethylsilane (TMS) signal at 0.0 ppm as a standard. The data are being reported as [s, singlet; d, doublet; t, triplet; m, multiplet or unresolved; brs, broad singlet, coupling constant(s) in hertz, integration). 13C NMR spectra were recorded on a Bruker AV-400 spectrometer and a Bruker AV-500 spectrometer in chloroform-d3. Chemical shifts are reported in ppm with the internal chloroform signal at 77.0 ppm as a standard. Mass spectra were recorded with Micromass QTOF2 Quadrupole/Time-of-Flight Tandem mass spectrometer using electron spray ionization.
1H nuclear magnetic resonance (NMR) spectra were recorded on a Bruker AV-400 spectrometer and a Bruker AV-500 spectrometer in chloroform-d3. Chemical shifts are reported in parts per million (ppm) with the internal tet-ramethylsilane (TMS) signal at 0.0 ppm as a standard. The data are being reported as [s, singlet; d, doublet; t, triplet; m, multiplet or unresolved; brs, broad singlet, coupling constant(s) in hertz, integration). 13C NMR spectra were recorded on a Bruker AV-400 spectrometer and a Bruker AV-500 spectrometer in chloroform-d3. Chemical shifts are reported in ppm with the internal chloroform signal at 77.0 ppm as a standard. Mass spectra were recorded with Micromass QTOF2 Quadrupole/Time-of-Flight Tandem mass spectrometer using electron spray ionization.
3
Spectroscopic Analysis of Organic Compounds
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Mass spectra were recorded with Micromass QTOF2Quadrupole/Time-of-Flight Tandem mass spectrometer (Milford, MA, USA) using electron spray ionization. 1H-NMR spectra were recorded on a Bruker AV-400 spectrometer (Bruker, Fällanden, Switzerland) and a Bruker AV-500 (Bruker, Fällanden, Switzerland) spectrometer in chloroform-d. Chemical shifts are reported in ppm with the internal TMS signal at 0.0 ppm as a standard. The data is being reported as (s = singlet, d = doublet, dd = doublet of doublets, t = triplet, dt = doublet of triplets, m = multiplet or unresolved, q = quartet, dq = doublet of quartets, brs = broad singlet, coupling constant(s) in Hz, integration). 13C-NMR spectra were recorded on a Bruker AV-400 spectrometer and a Bruker AV-500 spectrometer in chloroform-d. Chemical shifts are reported in ppm with the internal chloroform signal at 77.0 ppm as a standard.
4
NMR and MS Characterization of Compounds
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1H NMR spectra were recorded at 298 K using a Brüker AV-400 spectrometer at a frequency of 400 MHz and are reported as parts per million (ppm) using CD3CN (δH 1.94 ppm) as an internal reference. 13C NMR spectra were recorded at 298 K using a Brüker AV-400 spectrometer at a frequency of 100 MHz and are reported as parts per million (ppm) using CD3CN (δH 1.94 ppm) as an internal reference. The electronic spray ionization (ESI) mass spectra were obtained using an LCT Premier XE mass spectrometer.
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1H NMR spectra were recorded at 298 K using a Brüker AV-400 spectrometer at a frequency of 400 MHz and are reported as parts per million (ppm) using CD3CN (δH 1.94 ppm) as an internal reference. 13C NMR spectra were recorded at 298 K using a Brüker AV-400 spectrometer at a frequency of 100 MHz and are reported as parts per million (ppm) using CD3CN (δH 1.94 ppm) as an internal reference. The electronic spray ionization (ESI) mass spectra were obtained using an LCT Premier XE mass spectrometer.
5
Polymer Characterization by GPC, FT-IR, NMR, and TGA
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Weight-average molecular weights (Mw) and dispersity indices (Mz/Mw) of the polymers were estimated on a Waters gel permeation chromatography (GPC) system equipped with a Waters 1515 isocratic HPLC pump and Waters 2414 refractive index detector. Polystyrene standards were utilized, and THF was used as the eluent at a flow rate of 1.0 mL min−1. Fourier transform infrared (FT-IR) spectra were measured on a Bruker AV 400 spectrometer. 1H NMR spectra was measured on a Bruker AV 400 spectrometer. Thermogravimetric analysis (TGA) was carried out on a PerkinElmer STA 8000 at a heating rate of 10 °C min−1 under a nitrogen flow.
6
Purification and Characterization of Organic Compounds
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Unless otherwise noted, materials were obtained commercially and used without further purification. All the solvents were treated according to general methods. Flash column chromatography was performed over silica gel (300 to 400 mesh). See Supplementary Materials and Methods for experimental details.
1H NMR spectra were recorded on a Bruker AV-400 spectrometer and a Bruker AV-500 spectrometer in chloroform-d3. Chemical shifts are reported in parts per million (ppm) with the internal tetramethylsilane (TMS) signal at 0.0 ppm as a standard. The data are reported as follows: s = singlet, d = doublet, t = triplet, m = multiplet or unresolved, brs = broad singlet, coupling constant(s) in hertz, integration. 13C NMR spectra were recorded on a Bruker AV-400 spectrometer and a Bruker AV-500 spectrometer in chloroform-d3. Chemical shifts are reported in ppm with the internal chloroform signal at 77.0 ppm as a standard. Mass spectra were recorded with a Micromass quadrupole/time-of-flight tandem mass spectrometer using electron spray ionization.
1H NMR spectra were recorded on a Bruker AV-400 spectrometer and a Bruker AV-500 spectrometer in chloroform-d3. Chemical shifts are reported in parts per million (ppm) with the internal tetramethylsilane (TMS) signal at 0.0 ppm as a standard. The data are reported as follows: s = singlet, d = doublet, t = triplet, m = multiplet or unresolved, brs = broad singlet, coupling constant(s) in hertz, integration. 13C NMR spectra were recorded on a Bruker AV-400 spectrometer and a Bruker AV-500 spectrometer in chloroform-d3. Chemical shifts are reported in ppm with the internal chloroform signal at 77.0 ppm as a standard. Mass spectra were recorded with a Micromass quadrupole/time-of-flight tandem mass spectrometer using electron spray ionization.
7
Microwave-Assisted Synthesis of 2-Propyl-4H-3,1-Benzoxazinone
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All of the used reagents and solvents were purchased from Merck (Germany). Solvents were dried according to the literature when necessary. The purity of the new compounds was checked with TLC. Büchi (Switzerland) melting point apparatus was used; melting points were uncorrected. MW reactions were performed using a mini-lab microwave catalytic reactor WBFY-205, ZZKD, Henan, China. IR spectra were recorded on FT-IR Nicolet Impact 400D (Spectral lab Scientific Inc. Canada), in KBr pellets (n in cm -1 ). 1 H-and 13 C NMR spectra were obtained on Bruker at 400 and 100 MHz (Bruker AV400 spectrometer, Bruker, USA), resp., in CDCl 3 or DMSO-d 6 (d in ppm relative to Me 4 Si as the internal standard, J in Hz). DEPT135-NMR spectroscopy (Bruker AV400 spectrometer, Bruker, USA) was used where appropriate, to aid the assignment of signals in the 1 H-and 13 C NMR spectra. For HRMS (FAB+) JEOL JMS-SX 102A instrument (Jeol, Japan) was used. Syntheses 2-Propyl-4H-3,1-benzoxazinone (1) (link) was prepared according to literature (15) (link). (2) (link). -A mixture of 2-propyl-4H-3,1-benzoxazinone 1 (10 mmol, 1.89 g) and ammonium acetate (40 mmol, 3.08 g) was irradiated in MW bath reactor at 100 W and 120 °C for 2-5 min. The resulting crude was filtered off, washed with cold water and recrystallized from petrol ether to give compound 2.
8
Synthesis and Characterization of Doxorubicin-Loaded Micelles
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Nε-Carbobenzyloxy-l -lysine (Z-Lys, Macklin, 98%), p-toluenesulfonyl chloride (TsCl, Macklin, 99%), 4-hydroxy benzaldehyde (Macklin, 98%), triphosgene (Adamas, 99%), methoxypolyethylene glycols (MPEG, Mn = 2000 g mol−1, adamas), hyperbranched polyethyleneimine (PEI, Mn = 1800 g mol−1, adamas), doxorubicin hydrochloride (DOX·HCl, Adamas, 98%), the solvents THF, CH2Cl2 and DMF were used after expulsion of water. MPEG2000-C6H4CHO, and Z-Lys NCA were synthesized in advance referring to the previous articles.50,51 (link)1H NMR spectra were recorded on a Bruker AV 400 spectrometers with DMSO-d6 as solvent. Fourier transform-infrared (FTIR) spectrometer (Nicolet 560 infrared spectrometer) was used to record FTIR spectra at 25 °C, and the transmittance mode was used. Transmission electron microscopy (TEM) images were acquired from a JEM-1200EX microscope. Dynamic light scattering (DLS) was measured on Malvern Nanozetasizer to analyze the diameters and distribution of the micelles. The concentration of DOX was measured by UV-visible absorption spectra in absorbance mode against a standard curve and PerkinElmer LS-55 spectrofluorometer was employed to measure the fluorescence spectra (Scheme 1 ).
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Nε-Carbobenzyloxy-
9
Synthesis and Characterization of Urushiol Derivatives
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All AR solvents were used without special treatment. All the reactions were monitored by TLC on silica gel F254 plates (Qingdao Haiyang Inc., Qingdao, China) for detection of the spot. Silica-gel column chromatography was performed for purification of the products. MS data were obtained on an Agilent 7890 mass spectrometer. Nuclear magnetic resonance (NMR) spectra were measured on Bruker AV-300 or AV-400 spectrometers. Chemical shifts were expressed in delta (δ) units and coupling constants in Hz. The chemical shifts were reported in parts per million (ppm) and the following abbreviations were used: singlet (s), doublet (d), triplet (t), quartet (q), multiplet (m), and doublet of doublets (dd). The purity of all compounds (urushiol and its derivatives) was determined by HPLC (Shimadzu Co., Tokyo, Japan) and found to be in the 95–99% range.
10
Spectroscopic Characterization of Compounds
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All starting materials and solvents were purchased from commercial suppliers and used without purification, unless otherwise noted. 1H and 13C NMR spectra were measured on Bruker AV400 spectrometers with tetramethylsilane (TMS) as the internal standard. Chemical shifts were reported in δ (ppm). High-resolution mass spectra were obtained on HClASS XEVOG2XSQTof in the ESI mode (HR-ESI-MS). All the spectra were in Supplemental data .
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