NMR experiments were acquired following standard protocols as previously reported15 (link),16 (link). NMR samples were prepared by dissolving 10 mg RA in 500 μL in deuterated methanol CD3OD. Spectra were internally referenced to the singlet resonance of 4,4-dimethyl-4-silapentane-1-sulfonic acid (DSS) at 0 ppm. Spectra were recorded on a BRUKER AVANCE DRX 400 MHz NMR spectrometer. All spectra were recorded using a sample with a concentration of 1.6 mM at 300 K. The experiments used were COrrelation SpectroscopY (COSY), Nuclear Overhauser Effect SpectroscopY (NOESY), Heteronuclear Single Coherence Correlation (13C-HSQC), Heteronuclear Multiple Bond Correlation (13C-HMBC). 1D 1H NMR parameters included 2 s acquisition time, 1.5 s relaxation delay, 16 scans and a total time of 1 min. Variations on the 1D experiment include 1D NOE, selective decoupling solvent saturation and T1 determination. 1D 13C NMR parameters included 0.8 s acquisition time with proton decoupling, 2.0 s relaxation delay with NOE enhancement, 192 scans and a total time of 10 min. All 2D NMR experiments parameters included 1.5 s relaxation delay, 1 to 8 scans and a total time between 5 min and 1 h.
Drx 400 mhz nmr spectrometer
Manufactured by Bruker
Sourced in Germany
The DRX 400 MHz NMR spectrometer is a nuclear magnetic resonance (NMR) instrument manufactured by Bruker. It operates at a frequency of 400 MHz and is designed to perform high-resolution NMR spectroscopy analyses.
Automatically generated - may contain errors
Lab products found in correlation
Cary 50 bio spectrophotometer, by Agilent Technologies (1 mentions)
Emxplus, by Bruker (1 mentions)
Sm 4000 8, by Oxford Instruments (1 mentions)
J 815, by Jasco (1 mentions)
Isolera one flash purification system, by Biotage (1 mentions)
Av 400 mhz nmr spectrometer, by Bruker (1 mentions)
Precoated silica gel 60 f254, by Merck Group (1 mentions)
Avc 600 mhz nmr spectrometer, by Bruker (1 mentions)
6 protocols using drx 400 mhz nmr spectrometer
1
NMR Characterization of Retinoic Acid
2
Spectroscopic Analysis of Molecules
3
Purification and Characterization of Organic Compounds
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
All reagents and solvents were obtained from commercial sources and used without further purification. Proton (1H) spectra were recorded on a Bruker DRX-400 MHz NMR spectrometer or on a Bruker AV-400 MHz NMR spectrometer in deuterated solvents. Chemical shifts were reported in δ (ppm) and spin-spin coupling constants as J (Hz) values and signals are designated as follows: (s) singlet, (br-s) broad singlet, (d) doublet, (dd) doublet of doublet, (t) triplet, and (m) multiplet. Mass spectra (MS) were recorded on an Advion CMS mass spectrometer. Flash purification was conducted with a Biotage Isolera One flash purification system using HP-Sil (Biotage) or puriFlash columns (Interchim) and the solvent gradient indicated in the specific examples. Thin-layer chromatography (TLC) was carried out on silica gel plates with UV detection. Preparative thin-layer chromatography (Prep-TLC) was conducted with 0.5 mm or 1 mm silica gel plates (Analtech: Uniplate, F254) and the solvents indicated in the specific examples.
4
Synthesis and Characterization of 4-Thiazolidinone Conjugates
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
All the solvents and regents were purchased from Sigma Aldrich (Gillingham, UK) and they were used in the reactions without purification. The progress of each reaction was monitored by ascending thin layer chromatography (TLC) using TLC aluminum sheets, silica gel 60F254 precoated (Merck, Darmstadt, Germany), and locating the spots using UV light as the visualizing agent or iodine vapor. The melting points for the 4-thiazolidinone conjugates were carried out using an open capillary method and they are uncorrected. 1H NMR spectra were obtained on a Bruker DRX-400 MHz NMR spectrometer in DMSO-d6 (δ in ppm relative to tetramethylsilane (TMS) as an internal standard) and 13C NMR spectra were recorded (DMSO-d6) on a Bruker DRX-100 MHz spectrometer (Bruker BioSpin MRI GmbH, Ettlingen, Germany). High-resolution mass spectra (HRMS) were obtained using an Agilent 6520 (QTOF) ESI-HRMS model (Thermo Fisher Scientific, Waltham, MA, USA).
5
NMR Spectroscopy of Peptides
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
NMR spectra of peptides were collected
at 298 K on a Brüker AVC 600 MHz NMR spectrometer equipped
with a triple resonance cryoprobe. 31P NMR spectra were
recorded on a Brüker DRX 400 MHz NMR spectrometer equipped
with a BBO probe. Peptides were dissolved in buffer containing 5 mM
phosphate (pH 4.0, 6.5, 7.2, or 8.0) with 25 mM NaCl, 100 μM
TSP, and 90% H2O/10% D2O. 3JαN and 3JHP were determined directly from the 1-D 1H NMR
spectra and proton-coupled 31P NMR spectra, respectively.
at 298 K on a Brüker AVC 600 MHz NMR spectrometer equipped
with a triple resonance cryoprobe. 31P NMR spectra were
recorded on a Brüker DRX 400 MHz NMR spectrometer equipped
with a BBO probe. Peptides were dissolved in buffer containing 5 mM
phosphate (pH 4.0, 6.5, 7.2, or 8.0) with 25 mM NaCl, 100 μM
TSP, and 90% H2O/10% D2O. 3JαN and 3JHP were determined directly from the 1-D 1H NMR
spectra and proton-coupled 31P NMR spectra, respectively.
6
Synthesis and Characterization of Urethane Compounds
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Cyclohexyl isocyanate was reacted with n-butanol and sec-butanol at stoichiometric ratio and samples were subject to 1H-NMR analysis using chloroform-d as the solvent. Similarly, DBTBA (dibutyltin butoxy acetate) was first mixed with sec-butanol and then reacted with cyclohexyl isocyanate at (1:1:1) mole ratio to form urethane. Then the product was subject to 1H-NMR analysis using chloroform-d as a solvent. DBTBA was synthesised by reacting with DBTDA (dibutyltin diacetate) + DBTDB (dibutyltin dibutoxide) at a (1:1) mole ratio by heating at 60 °C overnight [30 ]. The product was used without further purification. More details of the preparation of these compounds are given in our previous publication [7 ].
NMR spectra were recorded on Bruker DRX 400 MHz NMR spectrometer at ambient temperature at 399.89 MHz (1H) with chemical shifts (δ, ppm) reported relative to the solvent peaks of the deuterated solvent.
NMR spectra were recorded on Bruker DRX 400 MHz NMR spectrometer at ambient temperature at 399.89 MHz (1H) with chemical shifts (δ, ppm) reported relative to the solvent peaks of the deuterated solvent.
About PubCompare
Our mission is to provide scientists with the largest repository of trustworthy protocols and intelligent analytical tools, thereby offering them extensive information to design robust protocols aimed at minimizing the risk of failures.
We believe that the most crucial aspect is to grant scientists access to a wide range of reliable sources and new useful tools that surpass human capabilities.
However, we trust in allowing scientists to determine how to construct their own protocols based on this information, as they are the experts in their field.
Ready to get started?
Sign up for free.
Registration takes 20 seconds.
Available from any computer
No download required
Revolutionizing how scientists
search and build protocols!