User:Andrew W Long/Notebook/Synthesis of Lipid Modulators/2015/10/26

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Purification of AL2 via Büchi Separator

  • The compound mostly dissolved in ethyl acetate. ~10mL of the soluble portion was run through the Büchi, and two clean peaks eluted relatively close to each other first, and a third peak eluted near the end. The method was designed to ramp from 0% EtOAc (100% hexane) to 100%EtOAc.
  • The three fractions were then rotovapped separately, and redissolved independently in LC-MS methanol. Fraction 1 was examined via MS, and the target peak was observed. A significant peak indicating the dimerization of the sulfur starting material was also seen.
  • The MS of fraction 2 showed the product in a notably higher ratio.
  • A TLC of fraction 2 was done, and it showed a great deal of purity.
  • For next time,
    • Filter remainder of starting solution of crude AL2 to remove as much of the insoluble dimer as possible
    • continued notes for next time are on the back of MS scan in lab. Finish later.