All reagents were purchased and used without further purification unless otherwise indicated. Progress of reactions was monitored using TLC visualized by UV lamp (254 nm) or KMnO4 developer. Column chromatography was performed using 300 mesh silica gel (Shanxi Nuotai Biological Technology Co., Ltd., Yuncheng, China). Melting points (m.p.) were measured on a Shenguang WRR melting point apparatus (Shanghai Shenguang Instrument Co., Ltd., Shanghai, China). 1H- and 13C-NMR spectra were recorded using an Agilent 400 MR (Agilent Technology, Santa Clara, CA, USA) in deuterated solvents. Chemicals shifts are reported in parts per million (δ ppm) relative to TMS or the solvent peak. Coupling constants (J) are expressed in hertz (Hz). High-resolution mass spectrometry (HRMS) analysis was performed using an Agilent 1290–6545B Q-TOF mass spectrometer (Agilent Technology, Singapore).
Agilent 400 mr
Manufactured by Agilent Technologies
Sourced in United States
The Agilent 400-MR is a nuclear magnetic resonance (NMR) spectrometer. It is designed to analyze the structure and composition of chemical samples by measuring the magnetic properties of their nuclei.
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Lab products found in correlation
Alugram xtra sil g uv254, by Macherey-Nagel (2 mentions)
Microtof 2, by Bruker (2 mentions)
Avance 600, by Bruker (1 mentions)
Chns o ea 1108, by Carlo Erba (1 mentions)
Dimethyl sulfoxide (dmso), by Avantor (1 mentions)
2400 series 2 chns o analyzer, by PerkinElmer (1 mentions)
Agilent 500 dd2, by Agilent Technologies (1 mentions)
7 protocols using agilent 400 mr
1
Characterization of Organic Compounds
2
NMR Analysis of Methanol-d4 Samples
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The NMR polarizer model is Agilent–400 MR (Santa Clara, CA, USA) and methanol-d4 was the solvent used in the testing process. The entire assay was performed with the same NMR probe: 1H–NMR, 13C–NMR, and 2D–NMR. The duration, sample-and-hold time, pulse, pulse width and frequency of 1H–NMR were 1.000 s, 2.556 s, 45 degrees, 6410.3 Hz and 399.79 MHz, respectively. The duration, sample-and-hold time, pulse, pulse width, frequency, hydrogen decoupling frequency and power of 13C–NMR are 1.000 s, 1.311 s, 45 degrees, 25,000 Hz, 100.53 MHz, 399.79 MHz and 38 dB, respectively. The duration, sample-and-hold time, pulse, pulse width, frequency, frequency of carbon decoupling and power of 2D–HSQC are 1.000 s, 0.150 s, 4807.7 Hz, 20,105.6 Hz, 399.79 MHz, 100.54 MHz and 38 dB, respectively [94 (link)].
3
Spectroscopic Characterization of Imidazolidin-2-one
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The 1 H NMR and 13C NMR spectra were recorded on Agilent 400-MR (400 MHz) and Bruker Avance-600 spectrometers (600 MHz) in CDCl3 or DMSO-d6 using tetramethylsilane (TMS) as internal standard. The chemical shifts were reported in δ scale, and constant J values are presented in Hz. IR spectra were recorded on a UR-20 instrument in Nujol and on an IR-200 Fourier-transform IR spectrometer (TermoNicolet, Waltham, MA, USA) with a resolution of 4 cm−1 (KBr pellets). Electrospray ionization (ESI) high-resolution mass spectra were recorded on a Bruker maXis instrument. Melting points were measured on an Electrothermal IA 9000 series device in glass capillaries. Elemental analysis was performed on a Carlo Erba device EA 1108CHNS-O. The TLC on Silufol UV-254 was used to follow the course of reactions. Compound purification was performed using short dry column or flash-chromatography on silica gel (60, Fluka, Honeywell Research Chemicals, Morris Plains, NJ, USA) [81 (link)]. Started indole derivatives were used as purchased from Sigma-Aldrich. The 5-Hydroxy-1-phenylimidazolidin-2-one, 1 was obtained according to the procedure [61 (link)]. Solvents were purified by standard methods.
4
Characterization of 3-Aminoisoxazolines and Derivatives
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1H and 13C NMR spectra were recorded on a 400 MHz spectrometer Agilent 400-MR (400.0 and 100.6 MHz for 1H and 13C, respectively; Agilent Technologies, Santa Clara, CA, USA) at r.t. in CDCl3; chemical shifts δ were measured with reference to the solvent (CDCl3, δH = 7.26 ppm, δC = 77.16 ppm). When necessary, assignments of signals in NMR spectra were made using 2D techniques. Accurate mass measurements (HRMS) were obtained on Bruker micrOTOF II (Bruker Daltonik GmbH, Bremen, Gemany) with electrospray ionization (ESI). Analytical thin-layer chromatography was carried out with silica gel plates supported on aluminum (ALUGRAM® Xtra SIL G/UV254, Macherey-Nagel, Duren, Germany); the detection was performed by a UV lamp (254 nm). Column chromatography was performed on silica gel (Silica 60, 0.015–0.04 mm, Macherey-Nagel, Duren, Germany). 3-Aminoisoxazolines 1 ,2 and compounds 3a–l were obtained via described methods [26 (link)]. All other starting materials were commercially available. All reagents except commercial products of satisfactory quality were purified according to literature procedures prior to use.
Stock solutions of the compounds with a concentration of 5 mM were prepared in DMSO (Amresco, Cleveland, OH, USA).
Stock solutions of the compounds with a concentration of 5 mM were prepared in DMSO (Amresco, Cleveland, OH, USA).
5
NMR Spectroscopy and Mass Spectrometry Protocol
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1H and 13C NMR spectra were recorded on a 400 MHz spectrometer Agilent 400-MR (Agilent Technologies, Santa Clara, CA, USA), 400.0 and 100.6 MHz for 1H and 13C, respectively, at r.t. (room temperature) in CDCl3 if not stated othewise; chemical shifts δ were measured with reference to the solvent (CDCl3, δH = 7.26 ppm, δC = 77.16 ppm). When necessary, assignments of signals in NMR spectra were made using 2D techniques. Accurate mass measurements (HRMS) were obtained on a Bruker micrOTOF II (Bruker Daltonics, Billerica, MA, USA) with electrospray ionization (ESI). Analytical thin-layer chromatography was carried out with silica gel plates supported on aluminum (Macherey-Nagel, ALUGRAM® Xtra SIL G/UV254); the detection was carried out using a UV lamp (254 nm). Column chromatography was performed on silica gel (Macherey-Nagel, Silica 60, 0.015–0.04 mm), Rf (retardation factors) and solvent systems are given for each compound. 4-Chloropyrimidines 2a [44 (link)], 2b [45 (link)], 2d [46 (link)], 2e [47 (link)], 4-fluoropyrimidine N-oxide 6 [43 (link)] and 2-methyl-3,5,6,7,8,9-hexahydro-4H-cyclohepta[d]pyrimidin-4-one [48 (link)] were obtained via the described methods. All other starting materials were commercially available. All reagents except commercial products of satisfactory quality were purified according to the literature procedures, prior to use.
6
Synthesis and Characterization of Tp Ms Cu(THF)
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General Methods. All procedures were performed in a glovebox under an inert atmosphere of dinitrogen or using standard Schlenk techniques. All substrates were purchased Please do not adjust margins Please do not adjust margins from Sigma-Aldrich and used without further purification. Solvents were dried and degassed before use. The Tp Ms Cu(THF) 4a complex was prepared according to literature methods. NMR spectra were recorded on Agilent 400 MR or Agilent 500 DD2, 1 H and 13 C NMR shifts are reported relative to tetramethylsilane. FT-IR spectra were collected on a Nicolet IR200 FTIR spectrometer. Elemental analyses were performed on a Perkin-Elmer Series II CHNS/O Analyzer 2400.
7
2H NMR Spectroscopy of Deuterium-Proton Decoupled Samples
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2 H NMR spectra (61.397 MHz) were acquired using the NMR spectrometer Agilent 400MR allowing the use of a lock channel for the observation of the deuterium-proton decoupled spectra and equipped with a 10 mm deuterium selective probe.
The duration of the 90°pulse for 2 H nuclei was 25 μs. The acquisition time of the free induction decay was at least 4 s and the relaxation delay between pulses was 1 s. The spectral width was 1100 Hz. Chemical shifts were measured with reference to the solvent (D 2 O -4.72 ppm, DMSO -2.47 ppm). Integral intensities of signals were determined by an iteration analysis of the total line shape taking into account the residual field inhomogeneity and phase distortions using the INTSPECT2 program. 32
The duration of the 90°pulse for 2 H nuclei was 25 μs. The acquisition time of the free induction decay was at least 4 s and the relaxation delay between pulses was 1 s. The spectral width was 1100 Hz. Chemical shifts were measured with reference to the solvent (D 2 O -4.72 ppm, DMSO -2.47 ppm). Integral intensities of signals were determined by an iteration analysis of the total line shape taking into account the residual field inhomogeneity and phase distortions using the INTSPECT2 program. 32
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