RU2004127582A - METHOD FOR PRODUCING CRYSTAL FORM I KABERGOLINA - Google Patents

METHOD FOR PRODUCING CRYSTAL FORM I KABERGOLINA Download PDF

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Publication number
RU2004127582A
RU2004127582A RU2004127582/04A RU2004127582A RU2004127582A RU 2004127582 A RU2004127582 A RU 2004127582A RU 2004127582/04 A RU2004127582/04 A RU 2004127582/04A RU 2004127582 A RU2004127582 A RU 2004127582A RU 2004127582 A RU2004127582 A RU 2004127582A
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Russia
Prior art keywords
cabergoline
solvate
toluene
gel
resulting
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RU2004127582/04A
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Russian (ru)
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RU2277536C2 (en
Inventor
Ахмад Й. ШЕЙХ (US)
Ахмад Й. ШЕЙХ
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Фармация Корпорейшн (Us)
Фармация Корпорейшн
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D457/00—Heterocyclic compounds containing indolo [4, 3-f, g] quinoline ring systems, e.g. derivatives of ergoline, of the formula:, e.g. lysergic acid
    • C07D457/04—Heterocyclic compounds containing indolo [4, 3-f, g] quinoline ring systems, e.g. derivatives of ergoline, of the formula:, e.g. lysergic acid with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 8
    • C07D457/06—Lysergic acid amides
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D457/00—Heterocyclic compounds containing indolo [4, 3-f, g] quinoline ring systems, e.g. derivatives of ergoline, of the formula:, e.g. lysergic acid
    • C07D457/04—Heterocyclic compounds containing indolo [4, 3-f, g] quinoline ring systems, e.g. derivatives of ergoline, of the formula:, e.g. lysergic acid with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 8

Claims (15)

1. Способ получения кристаллической формы I каберголина, который включает получение толуольного сольвата формы Х каберголина и его преобразование в кристаллическую форму I каберголина.1. A method of obtaining crystalline form I of cabergoline, which includes obtaining a toluene solvate of form X of cabergoline and its conversion into crystalline form I of cabergoline. 2. Способ по п.1, в котором получение толуольного сольвата формы Х включает растворение каберголина в подходящем количестве толуола, охлаждение и перемешивание полученного раствора, гашение полученного геля холодным гептаном или гексаном, сбор полученного сольвата формы Х каберголина, имеющего ПР, представленную на фиг.1, и превращение сольвата формы Х в форму I каберголина при хранении при комнатной температуре и/или сушкой.2. The method according to claim 1, in which the preparation of a toluene solvate of form X includes dissolving cabergoline in an appropriate amount of toluene, cooling and stirring the resulting solution, quenching the gel obtained with cold heptane or hexane, collecting the resulting solvate of form X of cabergoline having a PR shown in FIG. .1, and the conversion of the solvate of form X to form I of cabergoline when stored at room temperature and / or drying. 3. Способ по п.2, в котором подходящее количество толуола составляет от 2,5 до 4,0 г толуола на грамм каберголина.3. The method according to claim 2, in which a suitable amount of toluene is from 2.5 to 4.0 g of toluene per gram of cabergoline. 4. Способ по п.2, в котором подходящее количество толуола составляет 3,5 г толуола на грамм каберголина.4. The method according to claim 2, in which a suitable amount of toluene is 3.5 g of toluene per gram of cabergoline. 5. Способ по п.2, в котором каберголин, используемый в качестве исходного материала, является маслом, кристаллической формой или их смесью.5. The method according to claim 2, in which cabergoline used as a starting material is an oil, a crystalline form, or a mixture thereof. 6. Способ по п.2, в котором раствор каберголина в толуоле охлаждают до температуры ниже -10°С и перемешивают в течение ночи.6. The method according to claim 2, in which a solution of cabergoline in toluene is cooled to a temperature below -10 ° C and stirred overnight. 7. Способ по любому из пп.2-6, в котором полученный гель гасят холодным гептаном.7. The method according to any one of claims 2 to 6, in which the resulting gel is quenched with cold heptane. 8. Способ по. п.7, в котором холодный гептан добавляют в гель в количестве от 10 до 20 г гептана на грамм каберголина.8. The method according to. Claim 7, wherein cold heptane is added to the gel in an amount of 10 to 20 g of heptane per gram of cabergoline. 9. Способ по п.2, в котором окончательную сушку проводят нагреванием твердых веществ сольвата формы Х, понижением давления вокруг твердых веществ или их сочетанием.9. The method according to claim 2, in which the final drying is carried out by heating the solids of the solvate of form X, lowering the pressure around the solids, or a combination thereof. 10. Способ по п.2, отличающийся тем, что десольватирование и стадия сушки объединены.10. The method according to claim 2, characterized in that the desolvation and drying stage are combined. 11. Сольват формы Х каберголина, имеющий ПР, показанную на фиг.1.11. A solvate of Form X cabergoline having a PR shown in FIG. 1. 12. Сольват формы Х каберголина, имеющий отличительные пики порошковой рентгенограммы, показанные в таблице I:12. A solvate of Form X cabergoline having distinctive powder X-ray peaks shown in Table I: Таблица I
Данные рентгенограммы, форма ХTable I
X-ray data, form X Угол 2Angle 2 Интенсивность, циклов/секЧ1000Intensity, cycles / secCh1000 Интенсивность, %Intensity,% 7,9887,988 68996899 100,00100.00 10,93710,937 837837 11,9711.97 12,06712,067 477477 6,826.82 14,92714,927 22132213 31,6631.66 17,16217,162 26032603 37,2537.25 17,32017,320 31633163 45,2645.26 19,93819,938 855855 12,2212.22 21,07521,075 27202720 38,9238.92 23,89223,892 13711371 19,6119.61 26,77926,779 10861086 15,5415,54
13. Способ получения сольвата формы Х каберголина по любому из п.11 или 12, включающий растворение каберголина в подходящем количестве толуола, охлаждение и перемешивание полученного раствора, гашение полученного геля холодным гептаном или гексаном, сбор полученного сольвата формы Х каберголина.13. A method for producing a cabergoline Form X solvate according to any one of Claims 11 or 12, comprising dissolving cabergoline in a suitable amount of toluene, cooling and stirring the resulting solution, quenching the obtained gel with cold heptane or hexane, collecting the resulting cabergoline Form X solvate. 14. Способ по п.13, в котором полученный гель гасят холодным гептаном.14. The method according to item 13, in which the resulting gel is quenched with cold heptane. 15. Способ по п.14, в котором количество холодного гептана, добавляемое для гашения геля, составляет от 10 до 20 г на каждый грамм каберголина.15. The method according to 14, in which the amount of cold heptane added to quench the gel is from 10 to 20 g for each gram of cabergoline.
RU2004127582/04A 2002-03-15 2003-03-10 Method for preparing cabergolin crystalline form i, cabergolin form x solvate and method for its preparing RU2277536C2 (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US36456702P 2002-03-15 2002-03-15
US60/364,567 2002-03-15
US41025302P 2002-09-12 2002-09-12
US60/410,253 2002-09-12

Publications (2)

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RU2004127582A true RU2004127582A (en) 2006-01-27
RU2277536C2 RU2277536C2 (en) 2006-06-10

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EP (1) EP1507777A4 (en)
JP (1) JP2005520831A (en)
KR (1) KR100605794B1 (en)
CN (1) CN1642953A (en)
AU (1) AU2003224665A1 (en)
BR (1) BR0308472A (en)
CA (1) CA2478149A1 (en)
IL (1) IL163779A0 (en)
MX (1) MXPA04008935A (en)
PL (1) PL372371A1 (en)
RS (1) RS77704A (en)
RU (1) RU2277536C2 (en)
TW (1) TW200306312A (en)
WO (1) WO2003078392A2 (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IL155545A (en) 2003-04-21 2009-12-24 Finetech Pharmaceutical Ltd Solvate form of cabergoline
CA2525104A1 (en) * 2003-05-08 2004-11-25 Ivax Pharmaceuticals S.R.O. Polymorphs of cabergoline
GB0409785D0 (en) * 2004-04-30 2004-06-09 Resolution Chemicals Ltd Preparation of cabergoline
GB0515430D0 (en) * 2005-07-27 2005-08-31 Resolution Chemicals Ltd Preparation of cabergoline
US7339060B2 (en) 2005-03-23 2008-03-04 Resolution Chemicals, Ltd. Preparation of cabergoline
GB0505965D0 (en) 2005-03-23 2005-04-27 Resolution Chemicals Ltd Preparation of cabergoline
EP1953157A1 (en) 2007-01-31 2008-08-06 LEK Pharmaceuticals D.D. New crystal form of cabergoline

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US4526892A (en) * 1981-03-03 1985-07-02 Farmitalia Carlo Erba, S.P.A. Dimethylaminoalkyl-3-(ergoline-8'βcarbonyl)-ureas
GB0007308D0 (en) * 2000-03-24 2000-05-17 Pharmacia & Upjohn Spa Process for preparing crystalline form | of cabergoline
IL163520A0 (en) * 2002-03-15 2005-12-18 Pharmacia Italia Spa Process for preparing crystalline form i of cabergoline

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MXPA04008935A (en) 2004-11-26
AU2003224665A1 (en) 2003-09-29
BR0308472A (en) 2005-01-11
CN1642953A (en) 2005-07-20
KR20050002858A (en) 2005-01-10
WO2003078392A3 (en) 2003-12-11
KR100605794B1 (en) 2006-08-01
TW200306312A (en) 2003-11-16
IL163779A0 (en) 2005-12-18
WO2003078392A2 (en) 2003-09-25
RU2277536C2 (en) 2006-06-10
JP2005520831A (en) 2005-07-14
RS77704A (en) 2006-10-27
CA2478149A1 (en) 2003-09-25
EP1507777A4 (en) 2007-03-07
EP1507777A2 (en) 2005-02-23
PL372371A1 (en) 2005-07-25

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