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.
Flash column chromatography system
Manufactured by Biotage
The FLASH column chromatography system is a lab equipment product by Biotage. It is designed for the purification and separation of chemical compounds through the process of column chromatography.
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4 protocols using flash column chromatography system
1
Spectinomycin Synthesis and Characterization
2
Synthesis of Coumarin-Functionalized Compound
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Example 14
Potassium carbonate (38 mg, 0.28 mmol) was added to a solution of p-AA (61 mg, 0.28 mmol) in 1 ml of 1:1 THF/DMSO. A solution of 4-bromomethyl-6,7-dimethoxycoumarin (84 mg, 0.28 mmol) in 1 mL of DMSO was then added dropwise via syringe. The resultant mixture was allowed to stir under nitrogen atmosphere overnight. The reaction mixture was then quenched via addition of 2 mL of H2O, and the product was then extracted with EtOAc (3×). The combined organic layers were dried over Na2SO4, filtered, and concentrated under reduced pressure. The crude product was purified using a Biotage Isolera Flash Column Chromatography system with an eluent gradient of 50% to 80% EtOAc in hexanes, providing the product as a white solid (55 mg, 45% yield). 1H NMR was consistent with the desired product.
3
Spectinomycin Dihydrochloride Pentahydrate Synthesis
4
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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