Chiral purification is a very important
step in the production
of many products such as active pharmaceutical ingredients (API).
These procedures are typically limited to a maximum yield of 50%.
Methods that include a racemization method, such as Viedma ripening,
offer a theoretical yield of 100%. Racemic conglomerate formation
is a necessary condition for chiral purification processes that exploit
crystallization, such as Viedma ripening. This condition forms a limiting
factor because only 10% of the chiral organic molecules crystallize
in this way; the other 90% form racemic compounds. For two compounds
that crystallize as racemic compounds we demonstrate that salt formation
can transform these into racemic conglomerates and show that these
can subsequently be fully deracemized using Viedma ripening. Salt
formation thus promises to be a crystal engineering tool to significantly
extend the applicability of Viedma ripening.
Deterioration of crystal surfaces during removal from solution prior to observation poses a problem for ex situ (atomic force) microscopy studies. We use potash alum (KAl(SO 4 ) 2 •12H 2 O) crystals as a model system and investigate the variation of the following parameters: size, orientation, lifting rate, humidity, airflow, rinsing, and pollution. A model to describe the effects occurring during removal is developed and implications for other systems are presented to minimize the discrepancy between in situ and ex situ surfaces. This discrepancy is minimized for potash alum when a crystal is lifted slowly from its solution in a vertical position at a humidity below room humidity and in the absence of air flow.
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