The largest database of trusted experimental protocols

37 protocols using drx spectrometer

1

Spectroscopic Analysis of Organic Compounds

Check if the same lab product or an alternative is used in the 5 most similar protocols
All Melting points are corrected and were determined with a STUART SCIENTIFIC Melting Point Apparatus Model SMP3. The TLCs were carried out on Eastman Chromatogram Silica Gel Sheets (13181; 6060) with fluorescent indicator. A mixture of ethyl acetate and methylene chloride (1:1) was used as eluent and iodine was used as revelator for the chromatograms. The IR spectra were measured with a Fourier Transform Infrared spectrometer Brucker Alpha. The UV spectra were recorded with a JENWAY 6715 UV-Vis Spectrophotometer. Combustion analyses were carried out with a C, H, N, S Euro EA from Hekatech company, their results were found to be in good agreement (±0.3%) with the calculated values. EIMS spectra were recorded on a double focusing mass spectrometer (Varian MAT 311A). 1H-NMR spectra were recorded in DMSO-d6 on a Bruker DRX spectrometer operating at 500 MHz. 13C-NMR spectra were recorded in DMSO-d6 on a Bruker DRX spectrometer operating at 125 MHz. TMS was used as internal reference.
+ Open protocol
+ Expand
2

Detailed Procedure for Compound Purification

Check if the same lab product or an alternative is used in the 5 most similar protocols
All commercially available starting materials, reagents, and solvents were used without further purification unless otherwise stated. All reactions were monitored by TLC with 0.25 mm silica gel plates (60GF-254). UV light, iodine stain, and ferric chloride were used to visualize the spots. Silica gel or C18 silica gel was used for column chromatography purification. 1H and 13C NMR spectra were recorded on a Bruker DRX spectrometer at 600 MHz, with δ given in parts per million and J in hertz and using TMS as an internal standard. High-resolution mass spectra were conducted by Shandong Analysis and Test Center in Ji’nan, China. ESI-MS spectra were recorded on an API 4000 spectrometer. Melting points were determined uncorrected on an electrothermal melting point apparatus. All tested compounds are >95% pure by HPLC analysis, performed on a Agilent 1100 HPLC instrument using an 5 µm ODS HYPERSIL column (4.6 mm × 250 mm) according to the following methods. All target compounds were eluted with 35% acetonitrile/65% water (containing 0.1% acetic acid) over 20 min, with detection at 254 nm and a flow rate of 1.0 mL/min.
+ Open protocol
+ Expand
3

Characterization of Synthesized Compounds

Check if the same lab product or an alternative is used in the 5 most similar protocols
The melting points of the prepared compounds were determined on a Gallenkamp electronic apparatus. TLC was utilized to monitor the reactions’ progress and purity. The FT-IR spectra were recorded utilizing KBr discs on the FT-IR Jasco 4100 infrared spectrophotometer (λ, cm−1). NMR spectra were performed on the Bruker DRX Spectrometer (1H, 400 MHz and 13C, 100 MHz) in CDCl3 and DMSO-d6 using TMS as the internal standard. Mass spectra (m/z, %) were recorded on an Agilent Model 8890 spectrometer. Elemental analyses were determined utilizing the LECO Truspec Micro Analyzer (LECO, St. Joseph, MI, USA).
+ Open protocol
+ Expand
4

Quantitative NMR Analysis of Organic Compounds

Check if the same lab product or an alternative is used in the 5 most similar protocols
NMR spectra have been recorded at 14.09 T with a Bruker DRX spectrometer operating at 600 MHz equipped with a 5 mm reverse probe operating at room temperature. 1H-NMR spectra have been acquired quantitatively by using 128 scans with 8000 Hz of sweep width over 32 K points, at 298 K. 1H-13C heteronuclear bidimensional experiments, (SQC, HMBC) were recorded with 2 K and 256 data point for T2 and T1 dimensions. Direct and long-range heteronuclear coupling constants were set to 145 Hz and 8 Hz, respectively. Proton homocorrelated bidimensional experiments (TOCSY) were recorded using 2 K and 256 data point for T2 and T1 dimensions and mixing time was set to 90 ms. Chemical shifts are referred to 7.1 ppm and 77.3 ppm for 1H and 13C, respectively.
+ Open protocol
+ Expand
5

NMR Characterization and LC-MS Analysis

Check if the same lab product or an alternative is used in the 5 most similar protocols
All NMR spectra were recorded at ambient temperature on a 300 MHz Bruker DRX Spectrometer equipped with a 5 mm BBFO probe and a SampleExpress for automated sample handling. Proton (δH) chemical shifts are quoted in ppm and are internally referenced to the residual protonated solvent signal. Resonances are described as s (singlet), d (doublet), t (triplet) and so on. Coupling constants (J) are given in Hz and are rounded to the nearest 0.1 Hz.
Compound purity and identity were determined by LC–MS (Alliance 2795, Waters, Milford, MA). Purity was measured by UV absorbance at 210 nm. Mobile phase A consisted of 0.01% formic acid in water, while mobile phase B consisted of 0.01% formic acid in acetonitrile. The gradient ran from 5 to 95% mobile phase B over 1.75 min at 1.75 ml/min. An Agilent Poroshell 120 EC-C18, 2.7 µm, 3.0 × 30 mm column was used with column temperature maintained at 40 °C. 2.1 µL of sample solution were injected. RT refers to the retention time for the compound under the above conditions. Identity was determined on a SQ mass spectrometer by positive and negative electrospray ionization. m/z values are reported in Daltons, with the relevant fragment ions quoted in parentheses.
+ Open protocol
+ Expand
6

Weak Ligand Binding Detected by 19F NMR

Check if the same lab product or an alternative is used in the 5 most similar protocols
The weak affinity of the interactions we sought to measure places them outside the sensitivity limits of techniques to such as surface plasmon resonance (SPR), isothermal titration calorimetry (ITC), and differential scanning fluorimetry (DSF). The sensitivity problem is exacerbated for some of these techniques by the particularly small ligands (< 200 Da) and the relatively large protein (56,000 Da). We recognized that the problem of detecting very weak binding of a small ligand is reminiscent of the challenges faced in fragment-based drug discovery campaigns, and therefore borrowed an emerging tool from their repertoire, 19F NMR 24 (link), 25 (link).
19F NMR spectra were acquired on a Bruker DRX spectrometer equipped with an 11.7 T magnet (19F resonance frequency equals 470 MHz). 500 μM β-glycosidase in 50 mM phosphate buffer in H2O with 10% protonated DMSO, 2 mM 6-fluoroindole and 5 mM of the competitor ligand.
Protein samples were pre-treated with 2,4-dinitrophenyl 2-deoxy-2-fluoro-β-D-glucopyranoside. The 2,4-dinitrophenol serves as a leaving group such that the 2-deoxy-2-fluoro-β-D-glucose remains covalently attached to the protein. We confirmed labeling of the protein by broadening of the inhibitor’s 19F NMR peak, and also spectrophotometrically by production of 2,4-dinitrophenol.
+ Open protocol
+ Expand
7

Synthesis and Characterization of SAHA

Check if the same lab product or an alternative is used in the 5 most similar protocols
All materials and reagents used in this work were analytical reagents without further purification. SAHA was purchased from Melonepharma (Dalian, People’s Republic of China). Electrospray ionization mass spectrometry was determined on an API 4000 spectrometer. Nuclear Magnetic Resonance (NMR) spectra were obtained on a Bruker DRX spectrometer (400 MHz). The chemical shifts are defined as δ values (parts per million) relative to TMS internal standard. Significant 1H NMR data are reported in the following order: multiplicity (s, singlet; d, doublet; t, triplet; m, multiplet) number of protons. High-resolution mass spectrometer (HRMS) spectrums were conducted on an Agilent 6510 Quadrupole Time-of-Flight LC/MS deliver.
+ Open protocol
+ Expand
8

Synthesis and Characterization of Receptor L

Check if the same lab product or an alternative is used in the 5 most similar protocols
All of the materials used for synthesis were obtained from Sigma-Aldrich and used without further purification. All the solvents used were of analytical grade. Freshly de-ionized water was used throughout the experiment. The stock solutions of metal ions were prepared from their nitrate salts and the solutions of anions were prepared from their sodium salts. Elemental analysis was carried out on Elemental Vario MICRO cube analyzer. 1H NMR spectra were recorded on a Bruker DRX spectrometer operating at 400 MHz in CDCl3 and chemical shift were recorded in ppm relative to TMS. UV-visible spectra were recorded on a Shimadzu UV 1800 spectrophotometer using a 10 mm path length quartz cuvette with the wavelength in the range of 200–800 nm. Mass spectra were recorded on a Waters mass spectrometer using mixed solvent methanol and triple distilled water which was equipped with an ESI source. The pH measurements carried out using a digital pH meter (Merck). Both receptor L (1 × 10−5 M) and metal ions (1 × 10−4 M) solutions were prepared in CH3CN–H2O (1/1, v/v) and H2O respectively.
+ Open protocol
+ Expand
9

Analytical Characterization of Compounds

Check if the same lab product or an alternative is used in the 5 most similar protocols
All chemicals were obtained from commercial suppliers and used without further refinement. All reactions were detected by TLC using 0.25 mm silica gel plate (60GF-254). UV light and ferric chloride were used to show TLC spots. 1H NMR and 13 C NMR spectra were recorded on a Bruker DRX spectrometer at 500 MHz, using TMS as an internal standard. High-resolution mass spectra were recorded using a Thermo Scientific Q Exactive hybrid quadrupole-orbitrap mass spectrometer from Weifang Medical University.
+ Open protocol
+ Expand
10

Spectroscopic Characterization of Organic Compounds

Check if the same lab product or an alternative is used in the 5 most similar protocols
Infrared spectra were recorded
using a Shimadzu (FT-IR 8400S) FT-IR spectrophotometer using a KBr
disk. 1H and 13C NMR spectra were collected
at 400 and 100 MHz, respectively, on a Bruker DRX spectrometer using
CDCl3 and DMSO-d6 as solvents.
Elemental analyses were performed with an Elementar Vario EL III Carlo
Erba 1108 microanalyzer instrument. Melting point was recorded on
a Chemiline CL-725 melting point apparatus and was uncorrected. Thin-layer
chromatography (TLC) was performed using silica gel 60 F254 (Merck) plates.
+ Open protocol
+ Expand

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

Sign up now

Revolutionizing how scientists
search and build protocols!