ACI™ and Isolera™ Flash Systems

Time-Efficient Chemistry: Rapid Routes from Synthesis to Isolated Compound (II)

In order to obtain a fast synthesis of an N-unprotected tripeptide, microwave (mw) assisted deprotection, coupling and partial deprotection were applied starting with a purified protected dipeptide [Fig. 1]. The three consecutive mw assisted steps were performed without any intermediate purifications and were accomplished within some 30 minutes. The resulting crude mixture containing the Boc deprotected tripeptide ester was shown to be quite complex [Fig. 2]. The crude product was subjected to automated reversed phase flash chromatography, followed by automated fraction pooling and “thin film evaporation”. The total time for the entire procedure was 1 h 20 min. The purity of the product was > 99%.

Method Development in Flash Purification

Flash purification involves a simple liquid chromatography technique » Method development uses TLC as a way of deciding the parameters for the separation » Isocratic separations are easiest to develop, but gradient separations are more powerful » Software in the Isolera helps with conversion of an isocratic separation to a gradient » It is possible with the Spektra software to run step gradients » Loading options are dependent on the column type » SNAP offers the most flexibility » Care must be taken to choose the best loading option to get good purifications

Quick Guide to Isolera™

Preparation, How Much are You Purifying?

Flash Chromatography: Using UV Detection with UV Absorbing Mobile Phases

The UV absorption spectrum of some solvents overlaps with the product they dissolve, meaning that fraction collection processes cannot distinguish between solvent and product. Luckily, there is technology that solves this problem.

Isolera Software Upgrade Instructions

How to Install Isolera SW 2.3

New Flash System Capabilities Improve Purification Times and Performance

New, higher default flow rates enabled by Isolera ACI systems decreases purification times compared to other systems’ and cartridges’ default flow rate settings without sacrificing separation efficiency. Incorporation of gradient optimization by converting a linear gradient to a step gradient further reduces purification time and solvent use while maintaining separation integrity for a target molecule.

Isolera Assist Quick Guide

Organic Chemistry - Products from Start to Finish

Biotage has developed tools for every step of the organic process, with the entire workflow in mind. This dedicated suite of products vastly expands the range of options in order to truly accelerate discoveries of new molecules for future innovations.

Isolera™ Quick Guide

Isolera™ Release Notes

Isolera™ Installation and Safety

DMSO and DMF as Injection Solvents

DMSO and DMF are suitable injection solvents for reversed-phase flash purification. DMSO shows it can be loaded in larger volumes (up to 0.05 mL/g of C18 media or 3.5% of a column volume) without affecting chromatographic separations or carrying compounds with it.

Impact of Injection Solvent Choice on Peak Shape and Resolution in Reversed-phase Flash Chromatography

Reversed-phase chromatography is typically used when you need to separate several milligrams of relatively polar compounds that either are not soluble in normal-phase solvents or are not compatible with bare silica because they react, stick, or both. If you are currently using reversed-phase at preparative scale, such as flash chromatography, you know the mobile phase limitations – water with either methanol, acetonitrile, or THF. As with normal-phase flash chromatography, when it comes time to purify you want your crude sample fully solubilized in the weakest possible solvent at the highest possible concentration. ACS 2016

Options Available for Green Flash Chromatography

For those chemists performing organic synthesis, reaction mixture purification by flash column chromatography is an integral and necessary part of the synthesis process. However, flash chromatography consumes large volumes of solvent which either needs to be recycled or disposed. ACS 2016.