Spectinomycin dihydrochloride pentahydrate was purchased from Waterstone Technology (catalog number 81249, CAS number 22189-32-8, 95% in purity). All solvents used for chromatography and liquid chromatography were purchased from Aldrich. Flash column chromatography silica cartridges were obtained from Biotage Inc. Reactions were monitored by thin-layer chromatography (TLC) on pre-coated Merch 60 F254 silica gel plates and visualized using UV light (254 nm). A Biotage FLASH column chromatography system was used to purify mixtures. 1H NMR spectra were recorded on a Varian INOVA-500 spectrometer or on a Bruker 400 MHz NMR spectrometer. Chemical shifts (δ) are reported in parts per million relative to the residual solvent peak or internal standard (tetramethylsilane), and coupling constants (J) are reported in hertz (Hz). High resolution mass spectra were recorded on a Waters Xevo G2 QTOF LC–MS using ESI. Purity of the products was confirmed by UPLC/MS (the Waters Acquity). Elemental analysis was tested by Atlantic Microlab Inc. X-ray was analyzed on Bruker D8 diffractometer.
Inova 500 spectrometer
Manufactured by Bruker
Sourced in United States
The INOVA-500 is a high-performance nuclear magnetic resonance (NMR) spectrometer designed for advanced analytical and research applications. It features a 500 MHz superconducting magnet and provides reliable and consistent data acquisition for a variety of sample types and experimental protocols.
Automatically generated - may contain errors
Lab products found in correlation
400 mhz nmr spectrometer, by Bruker (3 mentions)
Flash column chromatography system, by Biotage (3 mentions)
Xevo g2 qtof lc ms, by Waters Corporation (3 mentions)
Uplc ms, by Waters Corporation (2 mentions)
D8 diffractometer, by Bruker (1 mentions)
8453 spectrophotometer, by Hewlett-Packard (1 mentions)
Avance 3 hd 400 spectrometer, by Bruker (1 mentions)
Avance 3 hd 300 spectrometer, by Bruker (1 mentions)
5 protocols using inova 500 spectrometer
1
Spectinomycin Synthesis and Characterization
2
Characterization of Organic Compounds
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The reagents and solvents were purchased from commercial suppliers and used without further purification. Deionized water was obtained from MilliQ (Burlington, MA, USA).
The NMR experiments were carried out on a Varian INOVA 500 spectrometer (Mundelein, IL, USA, 500 MHz for 1H and 125 MHz for 13C), on a Bruker 400 (400 MHz for 1H and 100 MHz for 13C), or on a Bruker 300 (300 MHz for 1H and 75 MHz for 13C). Chemical shifts were reported in parts per million using the solvent’s residual peak as the reference.
ATR FT-IR spectra were acquired using a JASCO 6200 device with a MIRacle Single Reflection ATR Diamond/ZnSe accessory. The samples were directly deposited onto the ATR sample holder, and the FT-IR spectra were collected. The raw IR data were processed with JASCO spectral manager software (Version 2).
UV–Vis absorption measurements were carried out on a Hewlett–Packard 8453 spectrophotometer (Palo Alto, CA, USA) with a controlled temperature system.
The NMR experiments were carried out on a Varian INOVA 500 spectrometer (Mundelein, IL, USA, 500 MHz for 1H and 125 MHz for 13C), on a Bruker 400 (400 MHz for 1H and 100 MHz for 13C), or on a Bruker 300 (300 MHz for 1H and 75 MHz for 13C). Chemical shifts were reported in parts per million using the solvent’s residual peak as the reference.
ATR FT-IR spectra were acquired using a JASCO 6200 device with a MIRacle Single Reflection ATR Diamond/ZnSe accessory. The samples were directly deposited onto the ATR sample holder, and the FT-IR spectra were collected. The raw IR data were processed with JASCO spectral manager software (Version 2).
UV–Vis absorption measurements were carried out on a Hewlett–Packard 8453 spectrophotometer (Palo Alto, CA, USA) with a controlled temperature system.
3
Spectinomycin Dihydrochloride Pentahydrate Synthesis
4
NMR Spectroscopy Protocols
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NMR experiments were carried out on a Varian INOVA 500 spectrometer (500 MHz for 1H and 125 MHz for 13C), on a Bruker Avance III HD 400 spectrometer (400 MHz for 1H and 100 MHz for 13C) or on a Bruker Avance III HD 300 spectrometer (300 MHz for 1H and 75 MHz for 13C) at 25 °C. Chemical shifts are reported in ppm using TMS as the reference.
5
Spectinomycin Dihydrochloride Pentahydrate Synthesis
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Spectinomycin dihydrochloride pentahydrate was purchased from Waterstone Technology (catalog number 81249, CAS number 22189-32-8, 95% in purity). All solvents used for chromatography and liquid chromatography were purchased from Aldrich. Flash column chromatography silica cartridges were obtained from Biotage Inc. Reactions were monitored by thin-layer chromatography on pre-coated Merch 60 F254 silica gel plates and visualized using UV light (254 nm). IR (neat) spectra were obtained using a Nicolet-iS5 FT-IR instrument. A Biotage FLASH column chromatography system was used to purify mixtures. 1H NMR spectra were recorded on a Varian INOVA-500 spectrometer or on a Bruker 400 MHz NMR spectrometer. Chemical shifts (δ) are reported in parts per million relative to the residual solvent peak or internal standard (tetramethylsilane), and coupling constants (J) are reported in hertz (Hz). High-resolution mass spectra were recorded on a Waters Xevo G2 QTOF LC–MS using ESI. Purity of the products was confirmed by UPLC/MS (the Waters Acquity). Spectral data for final compounds is given below, and data for intermediates are provided in Supplementary information.
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