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4 protocols using jms t100cs

1

NMR, IR, and Mass Spectroscopy Analysis

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The 1 H and 13 C NMR spectra were recorded on a JNM EX-270 (270 and 67.5 MHz), AL-400 (400 and 100 MHz), and a JNM ECA-600 spectrometer (600 and 150 MHz).
Chemical shifts were reported in ppm downfield from the peak of Me4Si (TMS) used as the internal standard. Splitting patterns are designed as "br, s, d, t, q, and m," indicating "broad, singlet, doublet, triplet, quartet, and multiplet," respectively. The IR spectra were recorded on a SHIMADZU IRPrestige-21 FT-IR spectrophotometer using a KBr disk or a NaCl cell. Mass spectra were obtained on a JEOL JMS-700 or a JEOL JMS-T100CS.
High-resolution mass spectra were obtained on a JEOL JMS-700 or a JEOL JMS-T100CS.
Column chromatography was performed on silica gel (Kanto Chemical Co.). Thin-layer chromatography was performed on pre-coated plates (0.25 mm, silica gel Merck 60 F254).
Reaction mixtures were stirred magnetically. Preparation of ku-76 and 2d were reported previously (Abe et al., 2012) (link).
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2

Characterization of Vanadium Compounds

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The cold-spray ionization mass spectra were recorded on a JEOL JMS-T100CS. NMR spectra were recorded with a JEOL JNM-LA400. 51V NMR spectra were measured at 105.15 MHz. Chemical shifts were referenced to VOCl3 (δ = 0 ppm) for 51V NMR. IR spectra were measured on a Jasco FT/IR-4100 using a nujol method. Elemental analyses of C, H, and N were performed by the Research Institute for Instrumental Analysis at Kanazawa University. GC analysis was performed on a Shimadzu GC-2014 with a flame ionization detector (FID) equipped with a ZB-WAXplus capillary column (phenomenex, internal diameter = 0.25 mm, length = 30 m), NEUTRABOND capillary column (GL science, internal diameter = 0.25 mm, length = 30 m), and ZB-5 capillary column (phenomenex, internal diameter = 0.25 mm, length = 30 m). Naphthalene was used as the internal standard. GC-MS spectra were measured on a Shimadzu GCMS-QP2010. UV/vis spectra were measured on a Jasco V-770.
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3

Spectroscopic Characterization of Fluorescent Probes

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1H-NMR spectra were recorded on a Bruker AVANCE III HD 400 MHz spectroscopy. Mass spectra were measured with a JMS-T100CS (JEOL), Waters SQD2 (Waters). Fluorescence spectra were measured on an FP-6300 fluorescence spectrophotometer (JASCO). Fluorescence images were obtained by LSM 800 confocal laser scanning microscopy (Zeiss), with excitation at 405 nm (for ECGreen), 561 nm (for LTR, RFP and PlasMem Bright Red), and 640 nm (for Mem Dye-Deep Red), using a 500–550-nm filter for ECGreen, a 550–650-nm filter for LTR, RFP and PasMem Bright Red, or a 640–760-nm filter for Mem Dye-Deep Red. Theoretical calculations were carried out using ChemOffice Professional 16 (PerkinElmer). HPLC analysis was performed under an isocratic condition (A: H2O containing 0.1% TFA, B: acetonitrile containing 0.1% TFA; A/B = 60/40) at a flow rate of 1 mL/min using an Inertsil ODS-3 column (250 × 4.6 mm, 5 μm) on a LC-20A (Shimadzu). Absorbance at 254 nm was monitored.
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4

Synthesis and Cytotoxicity Evaluation of Novel Imidazolium Ionic Liquids

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4-Butyl-3-methylimidazolium tetrafluoroborate (ionic liquids) was obtained from Shanghai Cheng Jie Chemical Co., Ltd. (China). 4-bromobenzaldehyde was purchased from Aladdin Reagent Co., Ltd. (China). Trimethylsilylacetylene (>98%) was obtained from Shanghai Rui Yi Medical Tech Co., Ltd. (China). Palladium (II) acetate (Pd(OAc)2), cuprous (Ι) iodide (CuI), triphenylphosphine (PPh3), and 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) were acquired from Sigma-Aldrich Chemical Co., (China). Column chromatography (CC): silica gel (100–200, or 200–300 mesh, Qingdao Marine Chemical Factory) was used for purification. The melting points (M.p.) of the newly synthesized compounds were tested on an WRR digital melting point apparatus. The 1H-NMR and 13C-NMR spectra were recorded on a Bruker AV-600 spectrometer, using tetramethylsilane (TMS) as an internal standard, δ in ppm, J in Hz. ESI-HRMS was collected with JEOL JMS-T100CS cold-spray time-of-flight mass spectrometer, in m/z. The enzyme-linked immunosorbent assay (ELISA) microplate-reader (Bio-Rad) was applied for cytotoxicity experiments.
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