FIELD: chemistry.
SUBSTANCE: invention relates to method of obtaining enriched with β-anomer 2'-desoxy-2',2'-difluorocytidine of formula (I)
, which includes stages: (i) interaction of enriched with α-anomer compound of 1-halogenribofuranose of formula (III) with nucleic base of formula (IV) in solvent obtaining enriched with β-anomer nucleoside of formula (II) , with constant removal of formed in reaction process silylhalogenide of formula R3SiX (V) by distillation using carrier or running inert gas through reaction mixture; and (ii) removal of protective group from enriched with β-anomer nucleoside of formula (II). Invention also relates to method of obtaining hydrate of enriched with β-anomer 2'-desoxy-2',2'-difluorocytidine of formula (I), which at stage (ii) after removal of protective group additionally includes stages of dissolving formula (I) nucleoside in water; heating of obtained solution to temperature from 40 to 60°C; cooling of solution to temperature ranging from 10 to 25°C with or without mixing and without changing pH; and filtering of deposited solid substances.
EFFECT: method improvement.
17 cl, 2 tbl, 7 ex
Title | Year | Author | Number |
---|---|---|---|
DERIVATIVES OF 1-α-HALOGEN-2,2-DIFLUORO-2-DEOXY-D-RIBOFURANOSE AND METHOD OF THEIR OBTAINMENT | 2005 |
|
RU2346948C2 |
METHOD OF OBTAINING DERIVATIVE OF D-ERYTHRO-2,2-DIFLUORO-2-DESOXY-1-OXORIBOSE | 2005 |
|
RU2337917C1 |
METHOD OF PREPARING BETA-ANOMER ENRICHED NUCLEOSIDES | 1993 |
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METHOD OF PRODUCING CAPECITABINE AND β-ANOMER RICH TRIALKYLCARBONATE COMPOUND USED THEREIN | 2008 |
|
RU2439064C1 |
SYNTHESIS OF β-L-2'-DESOXYNUCLEOSIDES | 2004 |
|
RU2361875C2 |
METHOD OF PURIFICATION AND RECOVERY OF 2'-DESOXY-2', 2'-DIFLUORONUCLEOSIDES | 1995 |
|
RU2161622C2 |
METHOD OF OBTAINING AND PURIFICATION GEMCITABINE HYDROCHLORIDE | 2006 |
|
RU2345087C2 |
METHOD OF PREPARING HEMCITABIN HYDROCHLORIDE | 1995 |
|
RU2154648C2 |
(S)-(-)-AMLODIPINE CAMSYLATE OR ITS HYDRATE AND PHARMACEUTICAL COMPOSITION INCLUDING THEM | 2007 |
|
RU2403241C1 |
METHODS OF PRODUCING 2'-FLUORO-2'-ALKYL-SUBSTITUTED OR OTHER SUBSTITUTED RIBOFURANOSYL PYRIMIDINES AND PURINES AND DERIVATIVES THEREOF | 2005 |
|
RU2433124C2 |
Authors
Dates
2009-07-10—Published
2005-12-29—Filed