All reactions were performed under an atmosphere of argon by using standard Schlenk or dry box techniques; solvents were dried over Na metal or CaH2 under nitrogen atmosphere. (R3P)AuCl (R = Me, Et) were synthesized using literature procedures66 (link)–68 (link). 1H, 13C, 29Si, and 31P NMR spectra were obtained with a Bruker AV 400 instrument at 400 MHz (1H NMR), 101 MHz (13C NMR) and 162 MHz (31P NMR), as well as Bruker AV 500 instrument at 500 MHz (1H NMR), 126 MHz (13C NMR), 99 MHz (29Si NMR), 202 MHz (31P NMR) at 298 K. Unless otherwise noted, the NMR spectra were recorded in benzene-d6 at ambient temperature. The 1H and 13C NMR chemical shifts were referenced to residual 1H and 13C signals of the solvents. NMR multiplicities are abbreviated as follows: s = singlet, d = doublet, t = triplet, dt = doublet of triplets, m = multiplet, and brs = broad singlet. Coupling constants J are given in Hz. Electrospray ionization (ESI) mass spectra were obtained at the Mass Spectrometry Laboratory at Hangzhou Normal University with a Bruker Daltonics MicroQtof spectrometer. Melting points were measured with a BUCHI Melting Point M-560. Sampling of air-sensitive compounds was carried out using a MBRAUN’s MB-10-G glove box. UV–Vis spectra were recorded on a Shimadzu UV-1800 spectrophotometer.
Melting point m 560
Manufactured by Büchi
The Melting Point M-560 is a laboratory instrument used to determine the melting point of solid samples. It features a temperature range from ambient to 400°C and can accommodate sample sizes up to 4mm in diameter. The unit provides accurate and reproducible results.
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Lab products found in correlation
Av 400 instrument, by Bruker (1 mentions)
Microqtof spectrometer, by Bruker (1 mentions)
Av500 instrument, by Bruker (1 mentions)
Uv 1800 spectrophotometer, by Shimadzu (1 mentions)
Tetrabutylammonium iodide, by Merck Group (1 mentions)
Pyridinium p toluenesulfonate, by Merck Group (1 mentions)
Ltq orbitrap xl, by Thermo Fisher Scientific (1 mentions)
Cesium carbonate, by Merck Group (1 mentions)
Ethyl acetate, by Merck Group (1 mentions)
Ftir spectrometer, by PerkinElmer (1 mentions)
Dpx 300, by Bruker (1 mentions)
Drx 400, by Bruker (1 mentions)
Drx 500, by Bruker (1 mentions)
Avance 3 hd 400, by Bruker (1 mentions)
Jnm ecx400p, by JEOL (1 mentions)
Silica gel 60 f254, by Merck Group (1 mentions)
Microtof q 2, by Bruker (1 mentions)
Ftir spectrophotometer, by PerkinElmer (1 mentions)
4 protocols using melting point m 560
1
Synthesis and Characterization of (R3P)AuCl Complexes
2
Functionalized Benzothiadiazole Synthesis
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All reagents and solvents were acquired from commercial courses using the highest available purity; BTO (95%, Fluorochem), ethyl acetate (≥99.8%, ChromAR®), pyridinium p-toluenesulfonate (≥99%, Sigma-Aldrich), silica for column chromatography (FlashPure 12 g, Büchi), acetone (≥99.5%, ChromAR®), by cesium carbonate (99%, Sigma-Aldrich), tetrabutylammonium iodide (≥99%, Sigma-Aldrich) High Resolution Mass Spectrometry (HRMS) and Fourier Transform Infrared Spectroscopy (FTIR). NMR and FTIR spectra and compounds’ characterization can be found in the SI. 1H and 13C NMR spectra were recorded on an Agilent Technologies 400 MHz NMR Premium Shielded Magnet using DMSO-d6 as solvent at room temperature. HRMS were measured with an Thermo LTQ Orbitrap XL with ESI ionization; samples were injected and eluted with 0.15 mL/min acetonitrile + 0.1% NH3. FTIR analyses were performed on Shimadzu IRTracer-100 equipment with ATR Specac Golden Gate KRS5. Melting points were determined with Büchi Melting Point M-560 equipment.
3
Characterization of Air-Sensitive Organometallic Compounds
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Where necessary, reactions were carried out under an inert argon atmosphere using standard Schlenk techniques. The solvents were dried by standard methods and freshly distilled before use. Et4NF⋅2 H2O, Ph4PCl, AgCl, and KF were commercially available.
The NMR spectra were, unless otherwise stated, recorded at ambient temperature on Bruker DPX 300, DRX 400, DRX 500, AVANCE III HD‐400, AVANCE III HD‐600 and AVANCE III HD‐700 spectrometers. The chemical shifts δ are given in ppm and referenced to tetramethylstannane (119Sn), and trichlorofluoromethane (19F) and tetramethylsilane (1H, 13C). Electrospray mass spectroscopy (ESI–MS) was recorded on a Thermoquest–Finnigan instrument using CH3CN as the mobile phase. The samples were introduced as solution in CH3CN through a syringe pump operating at 0.5 μL min−1. The capillary voltage was 4.5 kV, whereas the cone skimmer voltage was varied between 50 and 250 kV. Identification of the expected ions was assisted by comparison of experimental and calculated isotope distribution patterns. The m/z values reported correspond to those of the most intense peak in the corresponding isotope pattern. Elemental analyses were performed on a LECO‐CHNS‐932 analyzer. Melting points were determined using a Büchi Melting Point M‐560. IR spectra were recorded on a PerkinElmer FTIR spectrometer.
The NMR spectra were, unless otherwise stated, recorded at ambient temperature on Bruker DPX 300, DRX 400, DRX 500, AVANCE III HD‐400, AVANCE III HD‐600 and AVANCE III HD‐700 spectrometers. The chemical shifts δ are given in ppm and referenced to tetramethylstannane (119Sn), and trichlorofluoromethane (19F) and tetramethylsilane (1H, 13C). Electrospray mass spectroscopy (ESI–MS) was recorded on a Thermoquest–Finnigan instrument using CH3CN as the mobile phase. The samples were introduced as solution in CH3CN through a syringe pump operating at 0.5 μL min−1. The capillary voltage was 4.5 kV, whereas the cone skimmer voltage was varied between 50 and 250 kV. Identification of the expected ions was assisted by comparison of experimental and calculated isotope distribution patterns. The m/z values reported correspond to those of the most intense peak in the corresponding isotope pattern. Elemental analyses were performed on a LECO‐CHNS‐932 analyzer. Melting points were determined using a Büchi Melting Point M‐560. IR spectra were recorded on a PerkinElmer FTIR spectrometer.
4
Synthesis of Pyrazole Carbaldehydes
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All the chemicals used were purchased from Spectrochem, Avra and Sigma Aldrich and were used as received. Silica gel 60 F254 (Precoated aluminium plates) from Merck was used to monitor reaction progress. Melting points were determined on Buchi Melting Point M-560 apparatus and are uncorrected. IR (KBr) spectra were recorded on Perkin Elmer FTIR spectrophotometer and the values are expressed as νmax cm−1. The 1H and 13C spectra were recorded on Bruker top spin and Jeol JNM ECX-400P at 400 MHz and 100 MHz respectively. Mass spectra were recorded at Bruker Micro TOF Q-II. The chemical shift values are recorded on δ scale and the coupling constants (J) are in Hertz. Pyrazole carbaldehydes were prepared according to the procedure described in literature [48 (link)].
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