Reactions requiring an argon atmosphere were carried out using standard Schlenk techniques in a fume hood. Anhydrous diethyl ether was obtained from a dry solvent system and stored over 4 Å molecular sieves. All commercial materials were used as received without further purification. Microwave reactions were performed using a Biotage Initiator microwave reactor. Column chromatography was performed using a Biotage Isolera flash chromatography system. High-resolution mass spectra were collected on a JEOL AccuTOF 4G LC-plus equipped with an ionSense DART source. NMR spectra were recorded on a 500 MHz JEOL ECZ spectrometer. Chemical shifts δ are reported in ppm downfield from tetramethylsilane by referencing the spectra to residual solvent signals.
Isolera flash chromatography system
Manufactured by Biotage
The Isolera flash chromatography system is a automated purification platform designed for rapid and efficient separation and purification of chemical compounds. The system utilizes flash chromatography, a technique for separating and purifying mixtures of chemical compounds. The Isolera system automates the flash chromatography process, providing consistent and reliable results.
Automatically generated - may contain errors
3 protocols using isolera flash chromatography system
1
Anhydrous Ether Schlenk Synthesis
2
Cannabis Oil Purification by Flash Chromatography
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Example 2
In this example, a Biotage Isolera Flash Chromatography System was employed to process raw cannabis oil to deplete THC component. In particular, 45 g hemp oil (injection mass 6 wt %) was dissolved in 22.5 mL petroleum ether and injected to a 750 g normal phase silica gel column (SNAP KP-Sil 750 g, BIOTAGE) and rinsed with pet ether for a total injection volume of 67.5 mL. Solvent A was petroleum ether; Solvent B was 99.9% diethyl ether. Solvents A and B were employed to elute the column at 200 mL/min in a step gradient of 4 vol % B for 6 column volumes, then 8 vol % B for 4 column volumes, then 40 vol % B for 4 column volumes. Eluate was monitored at 220 nm and 240 nm. 120 mL fractions were collected. Following elution, the peak fractions were subjected to analytical HPLC or TLC analysis. Fractions 1-20 (1-6 CV) and 36-45 (11.5-14 CV) were combined and solvents removed by rotoevaporation. Analytical HPLC was employed to determine relative amounts of cannabinoids of interest.
3
Isolation and Characterization of Methyl Gamma Linolenate
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All chemicals used were purchased from Fluka chemicals. Their purity was checked by GC. All solvents were purified by distillation using Rotavap (Buchi R120) and if necessary residual water was removed. The components of solvents and elements are given in volume ratios of the components. Methyl gamma linolenate was isolated and purified by using Isolera Flash chromatography System (Biotage INC) and identified using different spectral and HPTLC techniques. The standard methyl gamma linolenate and routine were purchased from Sigma-Aldrich uses thin layer chromatography. The 1H NMR and 13C NMR were recorded on Bruker DRX-300 (300 MHz FT-NMR) using deuterated chloroform as solvent and TMS as internal standard. The mass spectra of compounds were recorded on JEOL GCMATE II GC-MS.
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