1H-, 13C-, and 31P-NMR spectra were recorded on Bruker DPX or Bruker AV NMR spectrometers operating at 400, 101, and 162 MHz, respectively. Small molecules were analyzed using a Waters TQD mass spectrometer equipped with a triple quadrupole analyzer. Samples were introduced to the mass spectrometer via an Acquity UltraPerformance Convergence Chromatography (UPC2) system, including a UPC2 Waters HSS C18 SB column (100 mm × 3.0 mm × 1.8 μm) gradient 90% CO2:10% methanol modifier (25 mM ammonium acetate) to 60% CO2:40% methanol modifier (25 mM ammonium acetate) in 3 min at a flow rate of 1.5 mL/min. The makeup flow (methanol/1% formic acid) was pumped at a flow rate of 0.45 mL/min into the mass spectrometer. Mass spectra were recorded using positive ion electrospray ionization.
Dibutylphthalate polystyrene xylene (dpx)
Manufactured by Bruker
Sourced in Germany
The DPX is a nuclear magnetic resonance (NMR) spectrometer designed for laboratory use. It is a versatile instrument that can be used for a wide range of NMR spectroscopy applications. The DPX provides accurate and reliable data acquisition and analysis for various sample types.
Automatically generated - may contain errors
Lab products found in correlation
Ultracentrifuge, by Merck Group (2 mentions)
Du 7400 spectrophotometer, by Beckman Coulter (2 mentions)
Ultrashield 400 mhz, by Bruker (2 mentions)
Avance 3 hd, by Bruker (2 mentions)
Hss c18 sb column, by Waters Corporation (1 mentions)
Tqd mass spectrometer, by Waters Corporation (1 mentions)
R axis rapid diffractometer, by Rigaku (1 mentions)
Ft ir 6300, by Jasco (1 mentions)
Q exactive, by Thermo Fisher Scientific (1 mentions)
Nicolet nexus 670 ftir, by Thermo Fisher Scientific (1 mentions)
Uv 1800 spectrophotometer, by Shimadzu (1 mentions)
R 210, by Büchi (1 mentions)
X8 prospector, by Bruker (1 mentions)
Rapid 2, by Bruker (1 mentions)
Tensor 27, by Bruker (1 mentions)
P 1010 polarimeter, by Jasco (1 mentions)
Kieselgel 60 f254, by Merck Group (1 mentions)
Isolera prime, by Biotage (1 mentions)
Topspin, by Bruker (1 mentions)
Spectrum bx, by PerkinElmer (1 mentions)
17 protocols using dibutylphthalate polystyrene xylene (dpx)
1
Comprehensive Spectroscopic Analysis of Small Molecules
2
Synthetic Protocols for Pyrazole and Formimidamide Derivatives
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Melting points were determined with a Sanyo (Gallenkamp)
instrument.
Infrared spectra were recorded using KBr pellets and a Jasco FT-IR
6300 instrument, and νmax was recorded in cm–1. 1H, and 13C NMR spectra were
evaluated with a Bruker DPX instrument at 600 MHz for 1H NMR and 100 MHz for 13C NMR and DMSO-d6 as a solvent, with TMS as an internal standard. Chemical
shifts are reported in d (parts per million). Mass
spectra were measured using a GCeMS DFS Thermo spectrometer in the
EI (70 eV) mode. The single crystal X-ray diffraction analysis was
made on the Rigaku R-AXIS RAPID diffractometer using filtered Mo Kα
radiation at −123 °C. The structure was solved by direct
methods, and the structure refinement was performed by SHELXL 2017/1.
All nonhydrogen atoms were refined anisotropically. The hydrogen atoms
were placed at calculated positions and refined using a riding model.
All solids were crystallized using the appropriate solvent (15.0 mL)
described in the experimental part, and the solids were heated at
60–65 °C (ethanol or ethanol/water) or at 35–40
°C (acetone) until they dissolved followed by filtering while
hot and then cooling. The 5-amino-1-phenyl-1H-pyrazole-4-carbonitrile8 (15 (link)) and N′,N″-(1,4-phenylene)-bis(N,N-dimethylformimidamide) 2 were prepared following
previously reported procedures.19 (link)
instrument.
Infrared spectra were recorded using KBr pellets and a Jasco FT-IR
6300 instrument, and νmax was recorded in cm–1. 1H, and 13C NMR spectra were
evaluated with a Bruker DPX instrument at 600 MHz for 1H NMR and 100 MHz for 13C NMR and DMSO-d6 as a solvent, with TMS as an internal standard. Chemical
shifts are reported in d (parts per million). Mass
spectra were measured using a GCeMS DFS Thermo spectrometer in the
EI (70 eV) mode. The single crystal X-ray diffraction analysis was
made on the Rigaku R-AXIS RAPID diffractometer using filtered Mo Kα
radiation at −123 °C. The structure was solved by direct
methods, and the structure refinement was performed by SHELXL 2017/1.
All nonhydrogen atoms were refined anisotropically. The hydrogen atoms
were placed at calculated positions and refined using a riding model.
All solids were crystallized using the appropriate solvent (15.0 mL)
described in the experimental part, and the solids were heated at
60–65 °C (ethanol or ethanol/water) or at 35–40
°C (acetone) until they dissolved followed by filtering while
hot and then cooling. The 5-amino-1-phenyl-1H-pyrazole-4-carbonitrile
previously reported procedures.19 (link)
3
Structural Characterization and Docking of C35 with PVY CP
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
All the chemical precursor materials used in the production of this article came from official sources. The melting points of all the target compounds were determined using an XGE X−4B micro melting point apparatus (Shanghai Yidian Physical Optics Instrument Co., Ltd., Shanghai, China). To identify the molecular structures, nuclear magnetic resonance NMR analyses were conducted using DMSO-d6 or CDCl3 as a solvent and a Bruker DPX instrument (Bruker, Karlsruhe, Germany) that was operated at a 400 or 500 MHz magnetic field strength. Then, a Thermo Scientific Q Exactive (Thermo Scientific, Waltham, MA, USA) was used and high-resolution mass spectrometry (HRMS) measurements were carried out. A 3D-QSAR model formulation was fulfilled utilizing SYBYL−2.0. In the experimental investigation, the software DISCOVERY STUDIO 4.5 (DS 4.5) was employed to execute the molecular docking of C35 and PVY CP.
4
NMR Spectroscopy Protocol
Check if the same lab product or an alternative is used in the 5 most similar protocols
1H and 13CNMR spectra were collected on a Bruker DPX operating at 300 MHz using TMS as an internal standard.
+ Expand
1H and 13CNMR spectra were collected on a Bruker DPX operating at 300 MHz using TMS as an internal standard.
5
Characterization of Synthesized Compounds
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
The melting points of the compounds were determined using an electric melting point apparatus (Toshniwal Pvt. Ltd., India) and the values were uncorrected. Thin layer chromatography (TLC) technique on silica gel-GF254 coated plates (Merck, Germany) is used for purity checking. Spots of TLC were recognized by iodine chamber. The ultraviolet (UV)-visible spectra of all the compounds were obtained at 200–400 nm using a double beam Shimadzu UV 1800 spectrophotometer at a concentration of 50 μg dissolved in methanol. The infrared (IR) spectra of synthesized compounds were recorded on a Thermo Nicolet Nexus 670-FTIR using KBr disc method with minimum forty scans. 1H-NMR spectra were obtained on Bruker UX-NMR instrument at 300 MHz, using tetramethylsilane as an internal standard and CDCl3 as a solvent, and chemical shift values were expressed in δ ppm. 13C NMR spectra were recorded on Bruker DPX at 300 Hz. The mass spectra were recorded on MASPEC (MSW/9629), and values were expressed as %relative abundance. Elemental analyses for synthesized compounds were carried over Perkin Elmer 240 CHN analyzer.
6
Analytical Techniques for Compound Characterization
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Ultraviolet (UV) and Mass spectra were taken on a DU® 7400 spectrophotometer (Beckman, München, Germany) and mass spectrometer (Thermo Quest Finnigan, San Jose, CA, USA) respectively. 1H and 13C Nuclear magnetic resonance (NMR) spectra were recorded on Ultrashield 400 MHz and 100 MHz spectrometer respectively (Bruker DPX, Faellanden, Germany). High performance Liquid chromatography (HPLC) analysis for compound analysis was carried out on Novapak C18 column (5 µm, 4.6 x 250 mm). Ultracentrifuge (Sigma, St. Louis, MO, USA), CO2 incubator (WTC Binder, Tuttlingen, Germany), Biosafety cabinet (Clean air, Chennai, India), autopipettes, ELISA plate reader (Labsystems, Helsinki, Finland) and Neubauer chamber (HBG, Gießen, Germany) were used for the cell culture. All extracts and fractions were concentrated using a vacuum rotary evaporator (Buchi R-210, Flawil, Switzerland).
7
NMR Analysis of Polysaccharide Sample
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
The dried polysaccharide sample (45 mg) was weighed, dissolved with 550 μL D2O (99.9 %), and transferred to a nuclear magnetic tube. 1D NMR (1H NMR, 13C NMR, DTPT-135°) and 2D NMR (1H–1H COSY, HSQC, HMBC, NOESY, TOCSY) spectra at room temperature were recorded by Bruker DPX.
8
Microwave-Assisted Synthesis of Privileged Scaffolds
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
All chemicals were purchased from Aldrich or Merck Companies. The 1H NMR (600 MHz) and 13C NMR (150 MHz) were run in a Bruker DPX instrument (δ ppm). Mass spectra were measured by using VG Autospec Q MS 30 and MS 9 (AEI) spectrometer, with EI (70 eV) mode. Melting points were recorded in a Gallenkamp melting point apparatus and are uncorrected. X-ray crystallographic structure determinations were performed by using Rigaku Rapid II and Bruker X8 Prospector single crystal X-ray diffractometers. The X-ray crystal structure data can be obtained free of charge from the Cambridge Crystallographic Data Centre via http://www.ccdc.cam.ac.uk CCDC1961565 for compound 4i . All reactions were monitored by TLC with 1:1 ethyl acetate/petroleum ether as eluent and were carried out until starting materials were completely consumed. After 7 min microwave irradiation was stopped and the reaction mixture was analyzed by TLC; after further irradiation of 5 min the reaction was complete (total reaction time 12 min).
9
NMR Spectroscopy for Chemical Analysis
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
1H and 13C solution
spectra were collected on a Bruker DPX operating at 300 MHz using
tetramethylsilane (TMS) as an internal standard.
spectra were collected on a Bruker DPX operating at 300 MHz using
tetramethylsilane (TMS) as an internal standard.
10
Characterization of Organic Compounds
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
All commercially available chemicals were purchased from Merck Company (Germany) and used without further purification. IR spectra were recorded from KBr disk using a FT-IR Bruker Tensor 27 instrument (USA). Melting points measured by using the capillary tube method with an electro thermal 9200 apparatus (Bibby Scientific Limited, Staffordshire, UK) are uncorrected. The 1H NMR (250 MHz) and 13C NMR (125 MHz) were run on a Bruker DPX (USA) at 250 MHz in CDCl3 and 125 MHz in D2O using tetramethylsilane as internal standard. GC-Mass analysis was performed on a GC-Mass model: 5973 network mass selective detector, GC 6890 Agilent Technologies (USA).
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!