1H NMR spectra were recorded on a Jeol RESONANCE ECZ 400S (400 MHz). Chemical shifts are reported in ppm from tetramethylsilane (TMS) with the solvent resonance resulting from incomplete deuteration as the internal reference (CDCl3: 7.26 ppm) or relative to TMS (δ 0.0). Data are reported as follows: chemical shift (ppm), multiplicity (s = singlet, d = doublet, t = triplet, q = quartet, br = broad, m = multiplet, dd = doublet of doublet, td = triplet of doublet), coupling constants (Hz), number of protons. 13C NMR spectra were recorded on a Jeol RESONANCE ECZ 400S (100 MHz) with complete proton decoupling. Chemical shifts are reported in ppm from tetramethylsilane with the solvent as the internal reference (CDCl3: 77.16 ppm). High-resolution mass spectrometry was performed on LCQ Fleet-Thermo Scientifics (Waltham, MA, USA). All reactants or reagents were purchased from Aldrich TCI, alfa aesar, and acros were directly used without further purifications. Silica gel column chromatography was performed with Silica Gel of Kieselgel 60 (Merck, KGaA, 64271 Darmstadt, Germany).
Ecz 400
Manufactured by JEOL
Sourced in Japan
The JEOL ECZ 400S is a high-performance nuclear magnetic resonance (NMR) spectrometer. It operates at a magnetic field strength of 9.4 Tesla, providing a 1H operating frequency of 400 MHz. The ECZ 400S is designed for advanced applications in chemical and materials analysis.
Automatically generated - may contain errors
Lab products found in correlation
Silica gel 60n, by Kanto Chemical (2 mentions)
Solarix ftms system, by Bruker (2 mentions)
Jmn ecs400, by JEOL (2 mentions)
Al 400, by JEOL (2 mentions)
Hybridit tof mass spectrometer, by Shimadzu (2 mentions)
Kieselgel 60 f254 plate, by Merck Group (1 mentions)
Agilent 1100 series, by Agilent Technologies (1 mentions)
Silica gel, by Qingdao Marine Chemical (1 mentions)
Silica gel 60, by Merck Group (1 mentions)
Kieselgel 60 f254, by Merck Group (1 mentions)
Uv 530 ultraviolet spectrophotometers, by Jasco (1 mentions)
Varian digilab fts 1000, by Agilent Technologies (1 mentions)
Apex 2 instrument, by Bruker (1 mentions)
L 2455 photodiode array detector, by Hitachi (1 mentions)
L 7100 pump, by Hitachi (1 mentions)
P 1010 polarimeter, by Jasco (1 mentions)
Lct premier xe waters, by Waters Corporation (1 mentions)
Jsx 3100rii, by JEOL (1 mentions)
Microflex lrf spectrometer, by Bruker (1 mentions)
Ftir 8400s spectrophotometer, by Shimadzu (1 mentions)
27 protocols using ecz 400
1
Spectroscopic Analysis of Organic Compounds
2
NMR Spectroscopy and Mass Spectrometry
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1H NMR spectra were recorded on a Jeol RESONANCE ECZ 400S (400 MHz). Chemical shifts are reported in ppm from tetramethylsilane (TMS) with the solvent resonance resulting from incomplete deuteration as the internal reference (CDCl3: 7.26 ppm) or relative to TMS (δ 0.0). Data are reported as follows: chemical shift, multiplicity (s = singlet, d = doublet, t = triplet, q = quartet, br = broad, m = multiplet, dd = doublet of doublet, td = triplet of doublet), coupling constants (Hz), number of protons. 13C NMR spectra were recorded on a Jeol RESONANCE ECZ 400S (100 MHz) with complete proton decoupling. Chemical shifts are reported in ppm from tetramethylsilane with the solvent as the internal reference (CDCl3: 77.16 ppm). High-resolution mass spectrometry was performed with on LCQ Fleet-Thermo Scientifics. All reactant or reagent was purchased from Aldrich, TCI, Alfa Aesar and Acros, and were directly used without further purifications. Silica gel column chromatography was performed with Silica Gel of Kieselgel 60 F254 plate (Merck).
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1H NMR spectra were recorded on a Jeol RESONANCE ECZ 400S (400 MHz). Chemical shifts are reported in ppm from tetramethylsilane (TMS) with the solvent resonance resulting from incomplete deuteration as the internal reference (CDCl3: 7.26 ppm) or relative to TMS (δ 0.0). Data are reported as follows: chemical shift, multiplicity (s = singlet, d = doublet, t = triplet, q = quartet, br = broad, m = multiplet, dd = doublet of doublet, td = triplet of doublet), coupling constants (Hz), number of protons. 13C NMR spectra were recorded on a Jeol RESONANCE ECZ 400S (100 MHz) with complete proton decoupling. Chemical shifts are reported in ppm from tetramethylsilane with the solvent as the internal reference (CDCl3: 77.16 ppm). High-resolution mass spectrometry was performed with on LCQ Fleet-Thermo Scientifics. All reactant or reagent was purchased from Aldrich, TCI, Alfa Aesar and Acros, and were directly used without further purifications. Silica gel column chromatography was performed with Silica Gel of Kieselgel 60 F254 plate (Merck).
3
Efficient Synthesis of Functionalized Compounds
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All reagents and anhydrous solvents are commercially available and were used without further purification. Temperatures are given in degrees Celsius (°C). NMR spectra were recorded on JEOL ECZ-400S spectrometers (JEOL, Ltd., Tokyo, Japan) using TMS (Tetramethylsilane) as the internal standard. The chemical shifts are reported in δ units (ppm) and the coupling constants (J) are in Hertz (Hz). The following multiplicity abbreviations are used: (s) singlet, (d) doublet, (t) triplet, (q) quartet, (m) multiplet, and (br) broad. ESIMS (Electrospray ionization-tandem mass spectrometry) data were measured on an Agilent 1100 Series (Agilent Technologies, Palo Alto, CA, USA). All reactions were monitored by TLC. Column chromatography was carried out using silica gel (Qingdao Marine chemical, Qingdao, China) with a 200~300 mesh size. Flash column chromatography was performed on a Biotage Isolera One (Uppsala, Sweden). Purity was determined by LCMS (Agilent Technologies, Palo Alto, CA, USA) and NMR spectroscopy (JEOL ECZ-400S, Tokyo, Japan). All of the final compounds were of purity higher than 95%.
4
Spectroscopic Characterization of Compounds
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Optical rotation spectra were recorded on a JASCO P-1010 polarimeter (JASCO, Tokyo, Japan). UV spectra were analyzed using JASCO UV-530 ultraviolet spectrophotometers. IR spectra were obtained on a Fourier-transform IR spectrophotometer Varian Digilab FTS 1000 (Varian Inc., Palo Alto, CA, USA). NMR spectra were obtained on a JEOL ECZ 400S or an ECZ 600R NMR (JEOL, Tokyo, Japan). HRESIMS data were collected on a Bruker APEX II instrument (Bruker Daltonik, Bremen, Germany). TLC was performed on Kieselgel 60 F254 (0.25 mm, Merck, Darmstadt, Germany) and/or RP-18 F254 (0.25 mm) coated plates and then visualized by spraying with 50% H2SO4 and heating on a hot plate. Silica gel 60 (Merck, 40−63 μm and 63−200 μm) were used for column chromatography. A Rheodyne 7725 injection port, a Hitachi L-2455 Photodiode Array Detector, and a Hitachi L-7100 pump (Hitachi, Tokyo, Japan), as well as a column Supelco Ascentis® C-18 Cat #: 581343-U, were applied for HPLC chromatography. All methods were carried out following the relevant guidelines and regulations.
5
Synthesis and Characterization of Thiosemicarbazide Derivatives
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General information: thiosemicarbazide, p-toluenesulfonic acid monohydrate, and all used substituted acetophenones were purchased from Sigma-Aldrich (Taufkirchen, Germany), while 96% ethanol and methanol were obtained from a local supplier (Avantor Performance Materials Poland S.A.). High-resolution mass spectra were obtained on an LCT Premier XE Waters apparatus, in positive electrospray ionization (ESI+) mode. The spectra were recorded on 600 MHz Bruker Avance and Jeol ECZ 400S spectrometers in DMSO-d6 as the solvent. Chemical shifts (δ) were reported in ppm relative to solvent signals (2.50 ppm and 39.52 ppm in 1H- and 13C-NMR spectra, respectively). The following abbreviations for multiplicity were used: s = singlet, d = doublet, t = triplet, q = quartet, quint = quintet, sext = sextet, hept = heptet, m = multiplet, and br = broad.
6
Comprehensive Nanomaterial Characterization Protocol
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Elemental analyses and electrospray-ionisation mass spectrometry (ESI-MS) were conducted at the analysis centre of Hokkaido University. The 1H NMR and 1H-1H COSY NMR spectra were acquired on a JEOL ECZ-400S or EX-270 spectrometer. Energy dispersive XRF spectra were acquired on a JEOL JSX-3100RII spectrometer using a Rh target. DLS analyses were conducted using an OTSUKA ELSZ-1000SCl analyser. Nitrogen and methanol vapour adsorption isotherms were measured using an automatic BELSORP-max (MicrotracBEL Co.) volumetric adsorption apparatus. Pore-size distributions were calculated using the density functional theory (DFT) method (DFT kernel: N2 at 77 K on silica, cylindrical pores, and NLDFT equilibrium model). Thermogravimetry-differential thermal analysis (TG-DTA) measurements were recorded using a Rigaku Thermoplus EVO TG-DTA 8120 with Al sample pans under an Ar flow. Matrix-assisted laser desorption/ionisation mass spectrometry (MALDI-MS) was conducted using a Bruker Microflex LRF spectrometer in a linear mode.
7
Synthesis and Characterization of 5-Arylselanyluracils
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All chromatographic separations were accomplished with Silica Gel 60N (Kanto Chemical Co., Inc.). Thin-layer chromatography (TLC) was performed with Macherey-Nagel Sil G25 UV254 pre-coated TLC plates. Reagents were used without further purification unless otherwise specified. Melting points were recorded on a Yanagimoto micro melting point hot-stage apparatus (MP-S3) and are not corrected. IR spectra were recorded on a SHIMADZU FTIR-8400S spectrophotometer and are reported in frequency of absorption (cm−1). Only selected IR peaks are reported. 1H NMR (TMS: δ = 0.00 ppm as an internal standard), 13C NMR (CDCl3: δ = 77.00 ppm as an internal standard), 19F NMR (trifluoromethylbenzene: δ = −64.0 ppm as an external standard) and 77Se NMR (Ph2Se2: δ = 436.15 ppm as an internal standard) spectra were recorded on a JEOL ECZ-400S (400 MHz, 100 MHz, 376 MHz and 76 MHz) spectrometer in CDCl3 unless otherwise stated. GC-MS (EI) spectra were recorded on Agilent 5977E Diff-SST MSD-230V spectrometer. HRMS (ESI) were recorded on Agilent 6230 Accurate-Mass TOF LC/MS system. The X-ray diffraction measurements carried out using a Rigaku XtaLAB Synergy, single source at home/near, HyPix3000 diffractometer. Spectroscopic data of 5-arylselanyluracils 5a, p, q, and 5s are in accordance with the literature.8,11,13 (link)
8
Synthesis and Characterization of LH20 Compound
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LH20 (98% purity, MW = 399.14) was synthesized as described previously [25 (link)], and a white solid powder was obtained. Briefly, the 2-chloro-5-fluoro-4-(4-fluoro-2-methoxyphenyl) pyrimidine intermediate was prepared using the Suzuki–Miyaura coupling reaction of commercial compounds (4-fluoro-2-methoxyphenyl) boronic acid and 2,4-dichloro-5-fluoropyrimidine with (dppf) Cl2 as the catalyst. This was followed by treatment with 4-morpholinopyridin-2-amine to afford the LH20 via the Buchwald–Hartwig amination reaction. The compound was tested using nuclear magnetic resonance (NMR, ECZ400S, JEOL, Tokyo, Japan) spectra. 1H NMR (400 MHz, CF3COOD) δ = 9.0 (d, J = 2.5, 1H), 8.1 (d, J = 7.4, 1H), 7.9–7.8 (m, 1H), 7.1 (ddt, J = 15.3, 7.8, 2.5, 3H), 6.8 (s, 1H), 4.2 (d, J = 4.9, 4H), 4.2–4.1 (m, 3H), 3.9 (d, J = 5.2, 4H). 13C NMR (100 MHz, CF3COOD) δ 160.75, 160.64, 158.49, 149.44, 146.46, 136.17, 133.69, 113.54, 109.36, 109.15, 104.97, 101.05, 100.79, 93.98, 65.73, 55.93, 45.86 (Figure 9 ). For cell experiments, a LH20 stock solution (20 mM) was prepared with DMSO (0.1%, Aladdin, Shanghai, China).
9
NMR Spectroscopy of Polymer-Li+ Interactions
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In an argon-filled glovebox, solutions of LiTFSI and polymers in ACN were prepared. The concentration of LiTFSI was kept constant at 50 mM in all solutions, while the polymer concentrations ranged between 0 and 2 M. The polymers studied were PEO, PCL and PTMC with M n = 4000 g mol À1 . The polymers were left overnight to dissolve in ACN under heating at 40 1C and stirring.
The NMR-titrations of Li + and Na + were conducted at 25 1C on a 400 MHz NMR spectrometer (JEOL ECZ 400S). The NMR titration experiment were performed by first measuring the 7 Li and 23
The NMR-titrations of Li + and Na + were conducted at 25 1C on a 400 MHz NMR spectrometer (JEOL ECZ 400S). The NMR titration experiment were performed by first measuring the 7 Li and 23
10
Characterization of Palladium Nanoparticles
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A 400 MHz NMR
spectrometer (ECZ400S, JEOL Ltd., Tokyo, Japan) was
used for 1H NMR spectra in CDCl3 with TMS (δ
= 0) as an internal standard. Inductively coupled plasma-atomic emission
spectroscopy (ICP-AES) was performed using ICPS-8100 (Shimadzu Co.,
Kyoto, Japan). A JEM 2100F transmission electron microscope (JEOL
Ltd., Tokyo, Japan) was used for investigation of Pd NPs. The samples
were prepared by placing a drop of the solution on carbon-coated copper
grids and allowed to dry in air. A Rigaku RINT 2500 diffractometer
(Cu Kα radiation) equipped with a monochromator was used for
powder XRDs. Polystyrene of narrow molecular weight distribution standards
and Pd(OAc)2 were purchased from Tosoh Co., Ltd. (Tokyo,
Japan) and Sigma-Aldrich Co. (Missouri, USA), respectively.
spectrometer (ECZ400S, JEOL Ltd., Tokyo, Japan) was
used for 1H NMR spectra in CDCl3 with TMS (δ
= 0) as an internal standard. Inductively coupled plasma-atomic emission
spectroscopy (ICP-AES) was performed using ICPS-8100 (Shimadzu Co.,
Kyoto, Japan). A JEM 2100F transmission electron microscope (JEOL
Ltd., Tokyo, Japan) was used for investigation of Pd NPs. The samples
were prepared by placing a drop of the solution on carbon-coated copper
grids and allowed to dry in air. A Rigaku RINT 2500 diffractometer
(Cu Kα radiation) equipped with a monochromator was used for
powder XRDs. Polystyrene of narrow molecular weight distribution standards
and Pd(OAc)2 were purchased from Tosoh Co., Ltd. (Tokyo,
Japan) and Sigma-Aldrich Co. (Missouri, USA), respectively.
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