If your email does not support graphics, please access the web version of this technical bulletin.  

 

 

CEOverture...

 

This month’s newsletter has a slightly different look to it from prior versions. In this installment we have gathered together a summary of recent advances in fluorous separation. We thought you would find the summary useful and informative, and indicative of how fluorous technology continues to evolve in exciting and practical ways. Be sure and read to the bottom to discover a tantalizing sales promotion. Well, a good deal, if not tantalizing…give us a try!

Cheers,

Phil

Philip E. Yeske
President & CEO

 

Advances in Fluorous Sorbent Technology


Since the publication of the first separation which combined a fluorous tagged molecule with a fluorous modified silica gel (J. Org. Chem. 1997, 62, 6714-6715) this technique has found widespread application in a number of fields.  In 2001 Fluorous Technologies, Inc. (FTI) began commercializing FluoroFlash® products and since that time the utility and robustness of fluorous separations have been demonstrated in labs around the world.  The separation of fluorous molecules from non-fluorous molecules using a FluoroFlash® stationary phase in a solid-phase extraction (SPE) has been found to be exceptionally predictable and robust.  Since that time, many customers asked for specific formats and applications that would further enhance their workflows.  In response we have developed alternative F-SPE separation modes to provide more options, allowing users of fluorous techniques greater flexibility.  FTI now offers a wide variety of preparative and analytical FluoroFlash® products designed to increase your productivity and help you get results.

 

Standard FluoroFlash® SPE silica gel and cartridges


Our standard cartridges are available in 2, 5, 10, and 20 gram cartridges which can be used with any commercially available SPE vacuum manifold unit.  These cartridges are commonly used for the purification of single reactions as well as small libraries and arrays ( a. Synlett 2001, 1488-1496.  b. Handbook of Fluorous Chemistry; Gladysz, J. A., Curran, D. P., Horvath, I. T., Eds.; Wiley-VCH: Weinheim, 2004, pp 101-127). The F-SPE is a general purification method which is essentially functional group independent.  This results in consistently higher product purities with less purification method development.  Applications of the technology include fluorous tagged reagents, fluorous tagged scavengers, and fluorous tagged library synthesis analogous to traditional solid phase synthesis.  By using fluorous molecules, however, you get all the benefits of solution phase chemistry (solution phase kinetics, complete reaction monitoring and analysis, precise control of stoichiometry, etc.).  Other advantages of the FluoroFlash® silica gel include high loading capacity (5-15%) and ease of recyclability (simply wash with MeOH or THF to regenerate the sorbent bed).

 

To learn more please see the F-SPE application note.

 

Fluorous Proteomics Applications


For those who conduct proteomics research and want to enrich protein and peptide mixtures using fluorous tagging techniques, the FluoroFlash® sorbent of choice is our 5 micron grade (catalog # 803-1100B) which is currently available unformatted in bulk.  We are beta-testing a pipette-tip format and nanocapillary HPLC columns.  If you're interested in either of these products, please let us know and we'll be happy to provide you a quote with special pricing.

 


24-Well Plate F-SPE


For researchers producing larger numbers of compounds, but in smaller quantities, the ability to purify multiple reactions at once is of prime importance.  As published last year (J .Comb. Chem. 2005, 7, 893-897), you can now use fluorous techniques to accomplish this in a 24 well format.  24 channel plateThe plate is packed with our standard 40 micron FluoroFlash® silica gel and the F-SPE can be conducted using a commercially available plate vacuum manifold (manufactured by Supelco, Fisher, and Waters). Overall throughput is further increased by the use of a multi-channel pipette for sample and solvent loading.  The receiving plate has a standard footprint that can be directly concentrated in a Genevac vacuum centrifuge.  Fluorous-based scavenging and amide bond forming reactions were reported with excellent purities and yields.  The 24 well format is ideally suited for parallel fluorous purification of reactions containing 10-100 mg of desired product.

 

If you would like to have 24 well plates packed for your parallel synthesis needs, please let us know.  We would be happy to provide a quote.

 

96 Deep-well Plate F-SPE and Gravity FluoroFlash® Silica Gel


For researchers producing libraries in the hundreds, the 24 well plate is still too limiting.  FTI has developed a solution to that issue by using a 96-deep well format.  Beyond just adding more wells, however, we have also developed a new grade of gravity filtration FluoroFlash® 96 well ex-blocksilica gel that doesn't require a vacuum manifold.  In addition, a new water-free protocol has been developed using DMSO as the fluorophobic wash.  Taken together, these developments enable true high throughput purification utilizing fluorous techniques. Within FTI labs we have conducted amide bond forming, scavenging, and Mitsunobu reactions and then separated the non-fluorous products from the fluorous by-products using the 96 deep-well plates with outstanding overall purities and recoveries. The 96 deep-well plate is suitable for reactions which yield 10-20 mg of product.  While we are still in the beta-testing period, if you are interested in evaluating the 96 deep-well plate or the gravity FluoroFlash® silica gel for yourself, please contact us.

 

Automated F-SPE


The incorporation of automated chromatography and SPE equipment has increased overall throughput and productivity in many labs.  The good news is that fluorous techniques are completely compatible with most of these systems.  By using fluorous methods in conjunction with automated systems, you get all the benefits of fluorous separations, i.e. little or no method development, high predictability, excellent separations, together with those from automation, including computer control, hands-free operation and automated fraction collection.  Fluorous separations have been conducted on Isco, Biotage, and Caliper systems.  FTI will be more than happy to help you format our FluoroFlash® sorbent to fit your instrument needs. 

 

Fluorous HPLC Columns and Fluorous TLC Plates


For separation of fluorous compounds by fluorous content or for the rapid development of F-SPE conditions, F-HPLC columns are essential.  FTI provides a wide range of column sizes from analytical to preparative.  Fluorous TLC plates, meanwhile, offer a quick and easy way to assess the retention of fluorous molecules on a fluorous modified surface.  Please see our website for application notes and details.

 

Fluorous Sorbent Sales Promotion


To encourage you to try fluorous purification techniques in your lab, we’re offering a great deal through the end of July on any of our standard sorbent products- just place a purchase order for sorbent products of more than $250 at list price and we’ll apply a 30% discount, plus we’ll throw in a free 10-pack of F-TLC plates (a $90 value!). Be sure to mention the Summer Sorbent Promotion when you order.

 

When you order your FluoroFlash® in the desired format, don't forget your fluorous reagents and tags!  Our online catalog has all the reagents and tags you need to try a wide range of chemistries. Looking for something not listed? Just let us know and we’d be happy to put a custom quote together for you- we do it all the time.