All commercial reagents and solvents were obtained from the commercial provider and used without further purification. Melting points (mp) were obtained with a MP90 melting point apparatus (Mettler-Toledo, Greifensee, Switzerland). 1H NMR and 13C NMR spectra were recorded on a Bruker Avance III 500 or II600 spectrometers (Varian, San Francisco, USA) in DMSO‑d6 with Me4Si as the internal standard. ESI high-resolution mass spectra (HRMS) were recorded on an Autospec Ultima-TOF spectrometer (Micromass UK Ltd., Manchester, U.K.). Flash chromatography over silica gel was performed on Combiflash Rf 200 (Teledyne, Nebraska, USA). Compounds 6a , 6b , 7a –c , 7l –o and 15b were synthesized and identified by mp or 1H NMR [[13] (link), [14] (link), [15] , [16] , [17] , [18] (link), [19] ].
Mp90 melting point apparatus
Manufactured by Mettler Toledo
Sourced in Switzerland
The MP90 melting point apparatus is a laboratory instrument used to determine the melting point of solid substances. It is designed to provide accurate and reliable measurements of the temperature at which a solid material transitions from a solid to a liquid state.
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Lab products found in correlation
Combiflash rf 200, by Teledyne (2 mentions)
Avance 3 500, by Agilent Technologies (1 mentions)
Microtof mass spectrometer, by Bruker (1 mentions)
P 2000 digital polarimeter, by Jasco (1 mentions)
J 810 spectropolarimeter, by Jasco (1 mentions)
Alpha spectrometer, by Bruker (1 mentions)
600 mhz instrument, by Bruker (1 mentions)
Combiflash rf 200 system, by Teledyne (1 mentions)
Avance 3 500, by Bruker (1 mentions)
5 protocols using mp90 melting point apparatus
1
Synthesis and Characterization of Novel Compounds
2
Spectroscopic Characterization of Organic Compounds
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All commercial solvents and reagents were used without any purification. All reactions were monitored by thin layer chromatography (TLC) and visualized under UV light at 254 nm or iodine fumigation. Melting points (mp) were obtained with a MP90 melting point apparatus (Mettler-Toledo, Greifensee, Switzerland). 1H and 13C NMR spectral data were recorded with a Bruker Avance 400, 500 or 600 spectrometers (Varian, San Francisco, USA) in DMSO‑d6 or CDCl3 using tetramethylsilane (TMS) as the internal standard. High-resolution mass spectrometry (HRMS) was performed on an AutospecUitima-TOF mass spectrometer (Micromass UK Ltd., Manchester, U.K.). The flash column chromatograms were conducted on silica gel (200–300 mesh) using Combiflash Rf 200 (Teledyne, NE, USA).
3
Physicochemical Characterization of Compounds
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Melting points were measured using a Mettler MP90 melting point apparatus, and reported as uncorrected. Optical rotation measurements were conducted by using a JASCO P-2000 digital polarimeter. UV and FT-IR spectra were recorded on an JASCO V-730 spectrophotometer and a Bruker Alpha spectrometer, respectively. Circular dichroism (CD) spectra were recorded on a JASCO J-810 spectropolarimeter. NMR spectra were recorded on a Bruker AV500D spectrometer. ESITOF MS data were obtained using a Bruker micrOTOF mass spectrometer. Column chromatography was performed using silica gel 60 (70–230 mesh ASTM, Merck). HPLC experiments were performed using a Dionex-Ultimate 3000 series instrument equipped with a binary pump, an autosampler, and a diode array detector.
4
Synthesis and Characterization of Aloperine
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All solvents and chemical reagents were used as purchased without any further treatment. Aloperine was purchased from the Yanchi Dushun Biological and Chemical Co. Ltd. (Shanxi, China), with the purity over 95%. Room temperature (rt) refers to 20–25 °C. Melting point (mp) was determined on MP90 melting point apparatus and was uncorrected (Mettler-Toledo, Greifensee, Switzerland). 1H-NMR and 13C-NMR spectra were recorded on a Avance 400 MHz or 500 MHz (Bruker, Zürich, Switzerland) and 600 MHz instruments (Bruker, Zürich, Switzerland), taking DMSO-d6 or CDCl3, as the solvent. ESI high-resolution mass spectrometry (ESI-HRMS) was performed on an AutospecUitima-TOF mass spectrometer (Micromass UK Ltd., Manchester, UK). Flash chromatography was performed on a Combiflash Rf 200 system (Teledyne, Lincoln, NE, USA).
5
Characterization of Novel Organic Compounds
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Unless otherwise noted, all commercial reagents and solvents were obtained from the commercial provider and used without further purification. Melting points (mp) were obtained with a MP90 melting point apparatus and were uncorrected (Mettler-Toledo, Greifensee, Switzerland). 1H-NMR and 13C-NMR spectra were recorded on a Bruker Avance III 500 (500 MHz for 1H-NMR; 126 MHz for 13C-NMR) spectrometer (Varian, San Francisco, CA, USA) with Me4Si as the internal standard. ESI high-resolution mass spectra (HRMS) were recorded on an Autospec Ultima-TOF spectrometer (Micromass UK Ltd., Manchester, UK). Flash chromatography was performed on a Combiflash Rf 200 system (Teledyne-Isco, Lincoln, NE, USA).
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