Improved Purification using Single StEP Columns
The Scripps Research Institute
Scott Harrison, Ben Pratt, K.C. Nicolaou http://www.scripps.edu/chem/nicolaou/

SINGLE StEP columns have given the ability to use flash chromatography for difficult separations. The SINGLE StEP columns have the ability to purify from 50mgs-20grams of compound. K.C. Nicolaou’s group at Scripps Institute has kindly provided detailed TLCs and pictures to show their separations, instead of crystallization or using glass columns. K.C. Nicolaou’s group has enhanced their work by using SINGLE StEP columns which are simple, use less solvent, take less time, higher productivity, and give them excellent separations.

 TLC Before                       TLC After  

 
1.2g scale, run hexane to 30% ethyle acetate (TLC is 20%) run on 25g column
   TLC Before                                    TLC After  

 
100 mg scale running 0 to 20% ethyl acetate (TLC is 20%) - orange spot is PhNMe2 run on 4g column

SINGLE StEP columns used on Biotage® SPD-1

Separations done on a Biotage® SPD-1 were kindly provided by Exelixis.
This TLC Plate A. indicated their are only 2 compounds separated. Fortunately the chemist used SINGLE StEP columns. This was a dirty mixture that resulted in 700mgs of pure material out of 772mgs possible. The below chromatogram run on a Biotage® shows 3 distinct bands. The invisible impurity by TLC was separated by SINGLE StEP columns 40g (4913119).
 

 TLC Before                                    TLC After

 
Crude Starting material 50% Hexane/Ethyle Acetate mixture only 2 spots shown.

SINGLE StEP Separations