RU2001111947A - METHODS FOR PRODUCING TRIGIDATE AND 4 D - (-) - TARTRATE SALT (1S, 2S) -1- (4-HYDROXYPHENYL) -2- (4-HYDROXY-4-Phenyl-PIPERIDIN-1-IL) -1-PROPANE - Google Patents

METHODS FOR PRODUCING TRIGIDATE AND 4 D - (-) - TARTRATE SALT (1S, 2S) -1- (4-HYDROXYPHENYL) -2- (4-HYDROXY-4-Phenyl-PIPERIDIN-1-IL) -1-PROPANE

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RU2001111947A
RU2001111947A RU2001111947/04A RU2001111947A RU2001111947A RU 2001111947 A RU2001111947 A RU 2001111947A RU 2001111947/04 A RU2001111947/04 A RU 2001111947/04A RU 2001111947 A RU2001111947 A RU 2001111947A RU 2001111947 A RU2001111947 A RU 2001111947A
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Prior art keywords
formula
compounds
tartrate salt
tartrate
aqueous methanol
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RU2001111947/04A
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Russian (ru)
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RU2203888C2 (en
Inventor
Джозеф Филип РЭЙНВИЛЛ
Терри Джин Мл. СИНЭЙ
Стэнли Уолтер ВАЛИНСКИ
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Пфайзер Продактс Инк.
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Claims (13)

1. Способ получения метансульфонат тригидрата соединения формулы (I):1. The method of producing methanesulfonate trihydrate of the compounds of formula (I):
Figure 00000001
Figure 00000001
 включающий следующие стадии: (i) растворение D-(-)-тартрата соединения формулы (I) в водном растворе метансульфоновой кислоты, и (ii) выделение из раствора соли - метансульфонат тригидрата.comprising the following steps: (i) dissolving the D - (-) - tartrate of the compound of formula (I) in an aqueous solution of methanesulfonic acid, and (ii) recovering from the salt solution methanesulfonate trihydrate. 2. Способ по п.1, отличающийся тем, что молярное соотношение метансульфоновой кислоты и D-(-)-тартратной соли соединения формулы (I) составляет 1,3-1,0.2. The method according to claim 1, characterized in that the molar ratio of methanesulfonic acid and D - (-) - tartrate salt of the compounds of formula (I) is 1.3-1.0. 3. Способ по п.1, отличающийся тем, что молярное соотношение метансульфоновой кислоты и D-(-)-тартратной соли соединения формулы (I) составляет 1,10-1,05.3. The method according to claim 1, characterized in that the molar ratio of methanesulfonic acid and D - (-) - tartrate salt of the compounds of formula (I) is 1.10-1.05. 4. Способ по п.1, отличающийся тем, что молярное соотношение метансульфоновой кислоты и D-(-)-тартратной соли соединения формулы (I) составляет 1,10-1,08.4. The method according to claim 1, characterized in that the molar ratio of methanesulfonic acid and D - (-) - tartrate salt of the compounds of formula (I) is 1.10-1.08. 5. Способ по п.1, отличающийся тем, что водная метансульфоновая кислота получена с использованием воды, не содержащей пироген.5. The method according to claim 1, characterized in that the aqueous methanesulfonic acid obtained using water that does not contain pyrogen. 6. Способ по п.1, отличающийся тем, что дополнительно включает следующие стадии: (i) растворения рацемической смеси, включающей соединения формул (I) и (II)6. The method according to claim 1, characterized in that it further includes the following steps: (i) dissolving the racemic mixture comprising the compounds of formulas (I) and (II)
Figure 00000002
Figure 00000002
 в водном метаноле в присутствии D-(-)-винной кислоты, и (ii) выделение D-(-)-тартратной соли соединения формулы (I) из раствора.in aqueous methanol in the presence of D - (-) - tartaric acid, and (ii) the isolation of the D - (-) - tartrate salt of the compound of formula (I) from solution. 7. Способ по п.5, отличающийся тем, что содержание воды в водном метаноле составляет 5-20%.7. The method according to claim 5, characterized in that the water content in aqueous methanol is 5-20%. 8. Способ по п.5, отличающийся тем, что содержание воды в водном метаноле составляет 7-10%.8. The method according to claim 5, characterized in that the water content in aqueous methanol is 7-10%. 9. Способ получения D-(-)-тартратной соли соединения формулы (I)9. The method of obtaining D - (-) - tartrate salt of the compounds of formula (I)
Figure 00000003
Figure 00000003
 включающие следующие стадии: (i) растворение рацемической смеси, включающей соединения формул (I) и (II):comprising the following steps: (i) dissolving a racemic mixture comprising compounds of formulas (I) and (II):
Figure 00000004
Figure 00000004
 в водном метаноле в присутствии D-(-)-винной кислоты, и (ii) выделение D-(-)-тартрата соединения формулы (I) из раствора.in aqueous methanol in the presence of D - (-) - tartaric acid, and (ii) the isolation of D - (-) - tartrate of the compound of formula (I) from solution. 10. Способ по п.9, отличающийся тем, что содержание воды в водном метаноле составляет 5-20%.10. The method according to claim 9, characterized in that the water content in aqueous methanol is 5-20%. 11. Способ по п.9, отличающийся тем, что содержание воды в водном метаноле составляет 7-10%.11. The method according to claim 9, characterized in that the water content in aqueous methanol is 7-10%. 12. D-(-)-тартратная соль соединения формулы (I)12. D - (-) - tartrate salt of the compounds of formula (I)
Figure 00000005
Figure 00000005
 где отношение (1S,2S)-энантиомера к его (1R,2R)-антиподу составляет более 97%.where the ratio of the (1S, 2S) enantiomer to its (1R, 2R) antipode is more than 97%. 13. Соль по п.10, отличающийся тем, что соотношение (1S,2S)-энантиомера к его (1R,2R)-антиподу составляет более 98%.13. The salt of claim 10, characterized in that the ratio of the (1S, 2S) enantiomer to its (1R, 2R) antipode is more than 98%.
RU2001111947/04A 2000-04-28 2001-04-27 Method of synthesis of (1s,2s)-1-(4-hydroxyphenyl)-2-(4-hydroxy-4- phenylpiperidin-1-yl)-1-propanol methanesulfonate trihydrate and d-(-)-tartrate salt RU2203888C2 (en)

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JP (2) JP3615496B2 (en)
KR (1) KR100442718B1 (en)
CN (2) CN1210262C (en)
AR (1) AR028376A1 (en)
AT (1) ATE277014T1 (en)
AU (1) AU781436B2 (en)
BR (1) BR0101630A (en)
CA (1) CA2345582C (en)
CZ (1) CZ20011471A3 (en)
DE (1) DE60105689T2 (en)
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ES (1) ES2227071T3 (en)
HK (1) HK1040246B (en)
HU (1) HUP0101723A3 (en)
ID (1) ID30006A (en)
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PL (1) PL347298A1 (en)
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SI (1) SI1151995T1 (en)
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AU7299301A (en) * 2000-06-21 2002-01-02 Bioarray Solutions Ltd Multianalyte molecular analysis using application-specific random particle arrays
US6743921B2 (en) 2002-01-24 2004-06-01 Dsm Catalytica Pharmaceuticals, Inc. Process for the preparation of nonracemic syn-1-(4-hydroxy-phenyl)-2-(4-hydroxy-4-phenyl-piperidin-1-yl)-1-propanol compounds
CA2545653C (en) * 2003-11-21 2014-07-08 Anp Technologies, Inc. Asymmetrically branched polymer conjugates and microarray assays
ATE496297T1 (en) 2005-05-02 2011-02-15 Anp Technologies Inc POLYMER CONJUGATE-ENHANCED BIOASSAYS

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DK0843661T3 (en) * 1995-08-11 2002-07-22 Pfizer (1S, 2S) -1- (4-hydroxyphenyl) -2- (4-hydroxy-4-phenyl-piperidin-1-yl) -1-propanol methanesulfonate trihydrate

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