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Objectives: development of supercritical diastereomer crystallization methods competitive in efficiency to the traditional solvent based crystallizations and having lower environmental effects.

Tasks and methodology:

  • Literature survey
  • Screening of promising resolving agents for all racemates (4 to 6). Selection of the two best pairs.
  • Measurement of solubility of the selected racemate(s) in CO2 and in CO2-solvent mixtures.
  • Development of the high pressure diastereomeric salt precipitation processes. (separately for the two pairs)
  • Critical evaluation and simple mathematical modelling of results. 

Results:

  • racemate – resolving agent pairs grouped to no salt / no enantioselectivity / poor enantioselectivity / good enantioselectivity groups
  • timeframe of salt formation mapped and analytical methodology developed
  • high pressure diastereomeric salt formation process developed and optimised

Dissemination: 2 papers in international journals, 1 paper in a national journal, 1 presentation at an international conference, 3 presentations at national conferences, 1 presentation at the conference of the doctoral school, involvement 2 times into the Open Day of the university.

Planned secondment: Rubotherm: 3 months, analysis of stability of diastereomers; Univesity of Valladolid: 3 months, feasibility studies on scale up of the developed process

 

Risk assessment: availability of suitable resolving agent might be critical. Cooperation initiated with organic chemical researches may help to overcome the problem if arises. 

   
© BME, Research Group on Supercritical Fluids, 2015