Crystalline form of the S-enantiomer of omeprazole

Drug – bio-affecting and body treating compositions – Designated organic active ingredient containing – Having -c- – wherein x is chalcogen – bonded directly to...

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5462737, A61K 3144, C07D40112

Patent

active

061628166

DESCRIPTION:

BRIEF SUMMARY
FIELD OF THE INVENTION

The invention provides a neutral form of the S-enantiomer of omeprazole which is S-5-methoxy-2-[[(4-methoxy-3,5-dimethyl-2-pyridinyl)-methyl]sulfinyl]-1H-b enzimidazole in a new physical form, more specifically in a solid state which can be at least partly crystalline, processes for preparing such a form of the S-enantiomer of omeprazole and pharmaceutical compositions containing it.


BACKGROUND OF THE INVENTION

The compound 5-methoxy-2-[[(4-methoxy-3,5-dimethyl-2-pyridinyl)methyl]sulfinyl]-1H-benz imidazole, having the generic name omeprazole, and therapeutically acceptable salts thereof, are described in EP 5129. The specific alkaline salts of omeprazole are disclosed in EP 124 495. Omeprazole is effective as a gastric acid secretion inhibitor, and is useful as an antiulcer agent. In a more general sense, omeprazole may be used for prevention and treatment of gastric-acid related diseases in mammals and especially in man.
Omeprazole is a sulfoxide and a chiral compound, wherein the sulfur atom being the stereogenic center. Thus, omeprazole is a racemic mixture of its two single enantiomers, the R-omeprazole and the S-omeprazole. The absolute configurations of the enantiomers of omeprazole have been determined by an X-ray study of an N akylated derivative of the (+)-enantiomer in neutral form. The (+)-enantiomer of the neutral form and the (-)-enantiomer of the neutral form were found to have the R and S configuration, respectively. The conditions for the optical rotation measurement for each of these enantiomers are described in WO 94/27988.
WO 92/08716 discloses R-omeprazole in its neutral form as an amorphous solid in Example 6. Different salts of the single enantiomers of omeprazole are described in WO 94/27988. The latter document discloses the preparation of the neutral form of the S-enantiomer of omeprazole in, for example, Example 10. However, it was obtained in the form of a syrup or oil which is unsuitable for pharmaceutical use because of the difficulty of handling an oil and incorporating it into solid pharmaceutical compositions, especially in a reproducible manner.


DESCRIPTION OF THE INVENTION

According to the invention there is provided S-omeprazole in a neutral form, i.e. not in the form of a salt, characterised in that the S-omeprazole is in a solid state.
Neutral S-omeprazole according to the invention is advantageous because it is more stable, easier to handle and store. It is also easier to characterise because it exists in a more well defined state, easier to purify and easier to synthesise in a reproducible manner.
S-Omeprazole according to the invention can in general be in an amorphous, partly crystalline or substantially crystalline solid state. Preferably it is in a partly crystalline solid state or a substantially crystalline solid state. More preferably it is in either of form A which is a crystalline form or form B which is a less crystalline form.


DETAILED DESCRIPTION OF THE DRAWINGS

FIG. 1 shows the X-ray powder diffraction pattern of neutral S-omeprazole in form A.
FIG. 2 shows the X-ray powder diffraction pattern of neutral S-omeprazole in form B.


DETAILED DESCRIPTION OF THE INVENTION

Forms A and B of S-omeprazole in neutral form are characterised by having X-ray powder diffraction patterns having the 20 degree angles, d-values and relative intensities given in Table 1.


TABLE 1 ______________________________________ Form A Form B Angle d-value, Relative Angle d-value, Relative .degree.20 .alpha..sup.1 (.ANG.) Intensity .degree.20 .alpha..sup.1 (.ANG.) Intensity ______________________________________ 5.78 15.29 Very strong 5.65 15.64 Strong 9.50 9.30 Weak 9.57 9.23 Medium 9.99 8.85 Weak 13.75 6.44 Medium 11.54 7.66 Weak 15.75 5.62 Medium 12.54 7.05 Weak 16.47 5.38 Medium 16.27 5.44 Strong 19.36 4.58 Weak 17.09 5.19 Strong 21.94 4.05 Weak 18.18 4.88 Weak 24.69 3.60 Weak 18.95 4.68 Strong 25.28 3.52 Weak 20.90 4.25 Medium 27.33 3.26 Weak 21.57 4.12 Medium 29.75 3.00 Very Weak

REFERENCES:
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patent: 4738974 (1988-04-01), Brandstrom
patent: 4786505 (1988-11-01), Lovgren et al.
patent: 5693818 (1997-12-01), von Unge
patent: 5714504 (1998-02-01), Lindberg et al.
patent: 5817338 (1998-10-01), Bergstrand et al.
patent: 5877192 (1999-03-01), Lindberg et al.
patent: 5900424 (1999-05-01), Kallstrom et al.
The Merck Index, Eleventh Edition, p. 1082, Ref. No. 6800, 1989.
Per Erlundsson, Journal of Chromatograhy, vol. 532, pp. 305-319, 1990.
von Unge, S. et al. "Stereochemical assignment of the enantiomers of omeprazole from X-ray analysis of a fenchyloxylmethyl derivative of (+)-(R)-omeprazole", Tetrahedron Asymmetry, vol. 8, No. 12, pp. 1967-1970 (1997).

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