Many microwave assisted organic synthesis (MAOS) reactions use polar solvents such as alcohols, DMF, DMSO, because they absorb and transfer microwave energy very efficiently. However, the downside of using polar, microwave absorbing solvents is that they can interfere with the flash chromatography that follows it injected directly onto a flash cartridge.
In this post, I discuss why dry loading can be advantageous when purifying polar-solvated reaction mixtures.
Continue reading When should I use dry loading instead of liquid loading with flash column chromatography?
Increasingly, organic and medicinal chemistry labs use mass-directed flash chromatography to isolate synthesized compounds. Mass-directed flash chromatography benefits are many, including collecting only the targeted molecule(s) in the reaction mixture. This approach simplifies compound purification since you know what you have made and it’s associated mass.
However, there are mass detection nuances that can be challenging. One of these is to know when an acid should be added to the mass detector’s make-up solvent to protonate targeted molecules. In this post, I will provide some insight on this topic.
Continue reading When should I add acid to my detector make-up solvent when using mass-directed flash chromatography?
Organic and medicinal chemists frequently utilize flash chromatography to purify their reaction mixtures. Normal-phase flash chromatography is most often used but may not the best methodology, especially when the compounds are quite polar and/or ionizable.
For these molecules, reversed-phase flash chromatography is preferred but often is not used due to an uncertainty regarding the best solvent choices and the reversed-phase mechanism. In this post, I will discuss how organic solvent choice in reversed-phase chromatography can influence the chromatographic separation.
Continue reading How does mobile phase organic solvent choice impact reversed-phase flash column chromatography?
In this post, I will look at the impact modifying mobile phase pH can have on reversed-phase separations.
Continue reading Using pH to optimize reversed-phase flash chromatography separations
Have you ever run flash column chromatography with mass detection (Flash-MS) and observed the total ion current or TIC increase during the purification only to find that there was no discernible compound contributing to the effect?
In this post I discuss how I came across this issue and the solution I found to work.
Continue reading How do I remove an annoying MS TIC background?
You have performed your synthesis and now it is time to purify the reaction mix. You have used thin-layer chromatography (TLC) and see a separation but when you try to purify with flash column chromatography, you can’t get the target compound separated from an impurity. So, what is happening (or isn’t happening)?
In this post I will give some input on why some separations are not transferrable from TLC.
Continue reading Why can’t I reproduce my TLC separation using flash column chromatography?