Search Results

You are looking at 1 - 3 of 3 items for :

  • Author or Editor: R. Peña x
  • Chemistry and Chemical Engineering x
  • Refine by Access: All Content x
Clear All Modify Search

Abstract  

The physicochemical characterization of the solid-state enantiomers and racemate of efaroxan hydrochloride (C13H17N2O+Cl-, M=252.5 g mol-1) was performed by thermoanalytical methods (differential scanning calorimetry, thermogravimetry and thermomicroscopy) and spectral methods (infrared spectrometry and X-ray diffractometry). The efaroxan enantiomers and racemate were shown to be unstable near the melting point. At the beginning of the decomposition, a loss of hydrogen chloride was observed. However when sealed pans were used, the compounds decomposed at higher temperature, allowing a precise evaluation of the melting enthalpies by means of differential scanning calorimetry. The nature of the racemate and its thermal stability were assessed by evaluating its free formation enthalpy. An enantiotropic solid-solid transformation (II→I) was noted for the racemate; the reverse process (I→II) follows zero-order kinetics.

Restricted access

Abstract  

The phase diagram of R(+)-S(-) efaroxan hydrochloride (Tfus.(R)=245.10.3C. ΔHfus.(R)=119.63.0 J g-1) shows a racemic compound. The melting temperature and melting enthalpy of the compound are: Tfus.(RS)=247.80.2C and ΔHfus. (RS)=124.62.4 J g-1. A solid ↔ solid transformation takes place at Ttrs.=1801C, ΔHtrs.=15.00.4 J g-1. This transition is observed between 3 and 97% R(+). The stability of the racemic compound already established in a previous study was confirmed by the value of Petterson's coefficient (i=1.19). The two eutectic positions at 20 and 80% R(+) that define the range over which the racemic compound is found, exclude the use of resolution methods by preferential crystallization.

Restricted access