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High-performance liquid chromatography for analytical and small-scale preparative separation of (R,S)-mexiletine using (S)-(—)-(N)-trifluoroacetyl-prolyl chloride and (1S)-(—)-camphanic chloride and recovery of native enantiomer by detagging

Dixit S., Dubey R., Bhushan R.

Acta Chromatographica

2014

Vol. 26, no. 4

625--636

A reversed phase high-performance liquid chromatographic method has been established for enantioseparation of (R, S)-mexiletine. Two volatile and thermally stable acyl chlorides, viz., (S)-(—)-(N)-trifluoro acetyl prolyl chloride and (1S)-(—)-camphanic chloride, were used as chiral derivatizing reagents. Binary composition of aqueous trifluoroacetic acid (0.1%)-acetonitrile as mobile phase was successful with ultraviolet (UV) detection at 210 nm. The method was optimized and validated for accuracy, precision, and limit of detection. The limit of detection was found to be 45 ng mL -1 and 80 ng mL -1 for the two types of diastereomers. Besides, kinetic resolution was achieved, and the experimental conditions optimized for this purpose provided diastereomeric excess up to 74% for (R)-isomer. On achieving a resolution value greater than 2, the optimized method for analytical enantioseparation was scaled-up to smallscale preparative level, and the native (R)-mexiletine was recovered by acid hydrolysis of the diastereomer.

Preliminary optimization of direct amination of 1-(2,6-dimethylphenoxy)-2-propanol. synthesis of 1-(2,6-dimethylphenoxy)-2-aminopropane

Leś A., Kajl M., Szelejewski W.

Polish Journal of Applied Chemistry

2005

Vol. 49, nr 3

195-203

Preliminary steps were reported of optimization of catalytic amination of 1-(2,6-dimethylophenoxy)-2-propanol in our new synthesis of 1-(2,6-dimethylphenoxy)-2-aminopropane (mexiletine). In our search for optimal conditions a series of experiments were performed based on the concept of fractional factorial design. A detailed statistical analysis of reaction responses indicated necessary modifications of the synthesis. Elevated temperatures and the use of a more efficient catalyst were found necessary in order to use direct amination in industrial synthesis of pharmaceutically important amine from commercially available alcohol.