269055-19-8Relevant articles and documents
Preparation method of etravirine chlorinated impurity
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Paragraph 0048-0049; 0056-0061, (2021/10/11)
The invention discloses a preparation method of an etravirine chlorinated impurity, which comprises the steps of dissolving etravirine in a dipolar solvent, adding hydrochloric acid with the mass fraction of 25-37%, heating to the temperature of 80-100 DEG C, reacting, adding water, crystallizing, and filtering to obtain an etravirine chlorinated impurity crude product; dissolving the etravirine chlorinated impurity crude product with an aprotic polar solvent, adding p-toluenesulfonic acid to form salt, and filtering to obtain etravirine chlorinated impurity p-toluenesulfonate; and dissolving etravirine chlorinated impurity p-toluenesulfonate with a corresponding aprotic polar solvent, adding alkali to dissociate the etravirine chlorinated impurity, adding water, crystallizing, filtering, washing with water, and drying to obtain the etravirine chlorinated impurity, wherein the etravirine chlorinated impurity is 4-[[6-amino-5-chloro-2-[(4-cyanophenyl) amino] pyrimidine-4-yl]-oxy]-3, 5-dimethyl benzonitrile. The preparation method disclosed by the invention is simple, relatively high in yield, mild in reaction condition and safe to operate, and the prepared impurity is relatively high in purity and can be used as a reference substance for research on the etravirine impurity.
RATE-CONTROLLED PARTICLES
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, (2008/06/13)
Rate-controlled particles, comprising compounds of the formula as a solid dispersion.