RS52423B - THE NEW CRYSTAL FORM OF AGOMELATIN, THE PROCEDURE FOR THE PRODUCTION OF IT AND THE PHARMACEUTICAL MIXTURES CONTAINING IT - Google Patents

THE NEW CRYSTAL FORM OF AGOMELATIN, THE PROCEDURE FOR THE PRODUCTION OF IT AND THE PHARMACEUTICAL MIXTURES CONTAINING IT

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RS52423B
RS52423B RS20120327A RSP20120327A RS52423B RS 52423 B RS52423 B RS 52423B RS 20120327 A RS20120327 A RS 20120327A RS P20120327 A RSP20120327 A RS P20120327A RS 52423 B RS52423 B RS 52423B
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agomelatine
production
expressed
formula
crystal form
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RS20120327A
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Serbian (sr)
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Jean-Claude Souvie
Gérard Coquerel
Julie Linol
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Les Laboratoires Servier
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Abstract

Kristalni oblik V agomelatina formule (I) :naznačen time što je dijagram difrakcije X zraka na dobijenom prašku kako sledi, a što je mereno na difraktometru Siemens D5005 (bakarna antikatoda) i izraženo kao među-mrežna udaljenost d, ugao Bragg 2 teta i, relativni intenzitet (izražen u procentima u odnosu na najintenzivniju prugu):2-teta (°) exp. d (A) exp. Intenzitet (%)9,84 8,979 1712,40 7,134 1513,31 6,646 co15,14 5,848 1815,98 5,543 1816,62 5,329 1917,95 4,939 10018,88 4,697 6520,49 4,332 2420,99 4,228 3423,07 3,852 3923,44 3,792 3624,28 3,663 5825,10 3,545 1926,02 3,422 1526,82 3,322 1927,51 3,239 16Prijava sadrži još 5 patentnih zahteva.Crystalline form V of agomelatine of formula (I): characterized in that the X-ray diffraction pattern on the obtained powder is as follows, measured on a Siemens D5005 diffractometer (copper anticathode) and expressed as inter-network distance d, Bragg 2 theta angle i, relative intensity (expressed as a percentage of the most intense band): 2-theta (°) exp. d (A) exp. Intensity (%) 9,84 8,979 1712,40 7,134 1513,31 6,646 co15,14 5,848 1815,98 5,543 1816,62 5,329 1917,95 4,939 10018,88 4,697 6520,49 4,332 2420,99 4,228 3423,07 3,852 3923, 44 3,792 3624,28 3,663 5825,10 3,545 1926,02 3,422 1526,82 3,322 1927,51 3,239 16The application contains 5 more claims.

Description

NOVI KRISTALNI V OBLIK NEW CRYSTAL V SHAPE

AGOMELATINA, POSTUPAK ZA AGOMELATIN, PROCEDURE FOR

NJEGOVU PROIZVODNJU I ITS PRODUCTION AND

FARMACEUTSKE SMEŠE KOJE GA PHARMACEUTICAL MIXTURES THAT CONTAIN IT

SADRŽE CONTENTS

Ovaj pronalazak se odnosi na novi oblik kristalnog V agomelatina ili A/-[2-(7-metoksi-1-naftil)etil]acetamida koji ima formulu (I): This invention relates to a new form of crystalline V agomelatine or N-[2-(7-methoxy-1-naphthyl)ethyl]acetamide having the formula (I):

na postupak za njegovu proizvodnju, kao i na farmaceutske smeše koje ga sadrže. to the procedure for its production, as well as to the pharmaceutical mixtures containing it.

Agomelatin ili /V-[2-(7-metoksi-1-naftil)etil]acetamid ima korisna farmakološka svojstva. Agomelatine or N-[2-(7-methoxy-1-naphthyl)ethyl]acetamide has beneficial pharmacological properties.

Ispoljava dejstvo dvostruke osobenosti, da je sa jedne strane agonist na receptorima melatoninergičnog sistema, a sa druge strane je antagonist receptora 5-HT2c- Ova svojstva mu daju aktivnost u centralnom nervnom sistemu i, preciznije, u lečenju opšte depresije, sezonskih depresija, poremećaja spavanja, kardiovaskularnih patologija, patologija digestivnog sistema, nesanica i umora kao posledica vremenske razlike, poremećaja apetita i gojaznosti. It exhibits the effect of a double peculiarity, that on the one hand it is an agonist on the receptors of the melatoninergic system, and on the other hand it is an antagonist of the 5-HT2c receptor. These properties give it activity in the central nervous system and, more precisely, in the treatment of general depression, seasonal depression, sleep disorders, cardiovascular pathologies, pathologies of the digestive system, insomnia and fatigue as a result of time difference, appetite disorders and obesity.

Agomelatin, njegova proizvodnja i njegova upotreba u terapeutske svrhe, opisani su u evropskom patentu EP 0 447 285. Agomelatine, its production and its use for therapeutic purposes are described in European patent EP 0 447 285.

Za procenu farmaceutske koristi od ovog jedinjenja, važno je njegovo dobijanje u vidu proizvoda odlične čistoće, a pre svega, u obliku savršene reproducibilnosti, koji ispoljava potrebna svojstva rastvorljivosti i olakšanog formulisanja čime omogućava produženo čuvanje bez posebnih uslova temperature, svetlosti, vlažnosti ili protoka kiseonika. To assess the pharmaceutical benefits of this compound, it is important to obtain it in the form of a product of excellent purity, and above all, in the form of perfect reproducibility, which exhibits the necessary properties of solubility and easy formulation, which allows for prolonged storage without special conditions of temperature, light, humidity or oxygen flow.

Patent EP 0 447 285 opisuje pristup od osam etapa do agomelatina, počevši od 7-metoksi-1-tetralona. Međutim, ovaj dokument ne precizira uslove dobijanja agomelatina u vidu jedne forme koja ispoljava svoje karakteristike na reproducibilan način. Zahtevalac sada ističe postupak dobijanja agomelatina u vidu kristalne forme koja je dobro definisana, savršeno reproducibilna i koja ispoljava korisne osobine dobrog rastvaranja i lakog formulisanja. EP 0 447 285 describes an eight-step approach to agomelatine, starting with 7-methoxy-1-tetralone. However, this document does not specify the conditions for obtaining agomelatine in the form of a single form that exhibits its characteristics in a reproducible manner. The applicant now highlights the process of obtaining agomelatine in the form of a crystalline form which is well defined, perfectly reproducible and which exhibits the useful properties of good dissolution and easy formulation.

Preciznije, ovaj pronalazak se odnosi na kristalni oblik V jedinjenja formule (I), koji je opisan dijagramom difrakcije X zraka praška, koji je izmeren na difraktometru Siemens D5005 (bakarna antikatoda) i izražen kao među-mrežna udaljenost d, ugao Bragg 2 teta i, relativni intenzitet (izražen u procentima u odnosu na najintenzivniju prugu): More specifically, this invention relates to the crystalline form V of the compound of formula (I), which is described by the X-ray powder diffraction pattern, which was measured on a Siemens D5005 diffractometer (copper anticathode) and expressed as inter-lattice distance d, Bragg angle 2 theta i, relative intensity (expressed as a percentage of the most intense line):

Pronalazak se, isto tako, odnosi na postupak za proizvodnju kristalnog V oblika jedinjenja formule (I), koji se odlikuje time što se agomelatin podvrgava mehaničkom mlevenju, nazvanom « visoko energetsko ». The invention also relates to the process for the production of the crystalline V form of the compound of formula (I), which is characterized by the fact that agomelatine is subjected to mechanical grinding, called "high energy".

Tokom postupka kristalizacije koji je u skladu sa pronalaskom, može se koristiti jedinjenje formule (I) koje je dobijeno ma kojim postupkom. During the crystallization process according to the invention, the compound of formula (I) obtained by any process can be used.

Pronalazak se, isto tako, odnosi na drugi postupak za proizvodnju kristalnog V oblika jedinjenja formule (I), koji se odlikuje time što se agomelatin greje sve dok se ne završi spajanje, zatim se ostavlja na temperaturi sredine i istovremeno se dodaje veoma mala količina kristalnog V oblika jedinjenja formule (I) koji je pripremljen svež, a zatim se ostavlja da se hladi sve dok se ne završi kristalizacija. The invention also relates to another process for the production of the crystalline V-form of the compound of formula (I), which is characterized by the fact that agomelatine is heated until the coupling is complete, then left at ambient temperature and at the same time a very small amount of the crystalline V-form of the compound of formula (I) is added, which is prepared fresh, and then allowed to cool until the crystallization is completed.

Poželjno, tokom ovog drugog postupka kristalizacije koji je u skladu sa pronalaskom, agomelatin će se topiti na 110°C. Preferably, during this second crystallization process according to the invention, the agomelatine will melt at 110°C.

Količina kristalnog V oblika koji se dodaje u toku ovog drugog postupka kristalizacije koji je u skladu sa pronalaskom, poželjno će biti između 1/100 do 1/50 težine agomelatina. The amount of crystalline V form added during this second crystallization process according to the invention will preferably be between 1/100 to 1/50 of the weight of agomelatine.

U toku ovog drugog postupka kristalizacije koji je u skladu sa pronalaskom, može se koristiti jedinjenje formule (I) dobijeno ma kojim postupkom. In the course of this second crystallization process which is in accordance with the invention, the compound of formula (I) obtained by any process can be used.

Dobijanje ove kristalne forme ima prednost što omogućava proizvodnju farmaceutskih formulacija koje imaju stalan i reproducibilan sastav, a ispoljavaju posebno korisna svojstva pri rastvaranju, što je naročito važno zbog toga što su ove formulacije namenjene oralnom primenjivanju. Obtaining this crystalline form has the advantage that it enables the production of pharmaceutical formulations that have a constant and reproducible composition, and exhibit particularly useful dissolution properties, which is particularly important because these formulations are intended for oral administration.

Farmakološko ispitivanje ovako dobijene forme V pokazalo je njenu značajnu aktivnost u centralnom nervnom sistemu, kao i na mikrocirkulaciju što omogućava njeno korišćenje za lečenje: stresa, poremećaja spavanja, anksioznosti, opšte depresije, sezonskih depresija, kardiovaskularnih patologija, patologija digestivnog sistema, nesanice i umora kao posledice vremenskih razlika, šizofrenije, napada panike, melanholije, poremećaja apetita, gojaznosti, nesanice, bola, psihotičnih poremećaja, epilepsije, dijabetesa, Parkinsonove bolesti, senilne demencije, raznih poremećaja koji su posledica normalnog ili patološkog starenja, migrene, gubitka pamćenja, Alchajmerove bolesti, kao i za poremećaje cerebralne cirkulacije. U drugom domenu aktivnosti, moguće je kristalnu formu V agomelatina korititi za tretman seksualnih disfunkcionalnosti, kao inhibitora ovulacije, imunomodulatora u tretmanu kancera. Pharmacological examination of the obtained form V showed its significant activity in the central nervous system, as well as on the microcirculation, which allows its use for the treatment of: stress, sleep disorders, anxiety, general depression, seasonal depression, cardiovascular pathologies, digestive system pathologies, insomnia and fatigue as a result of time differences, schizophrenia, panic attacks, melancholia, appetite disorders, obesity, insomnia, pain, psychotic disorders, epilepsy, diabetes, Parkinson's disease, senile dementia, various disorders resulting from normal or pathological aging, migraine, memory loss, Alzheimer's disease, as well as cerebral circulation disorders. In another domain of activity, it is possible to use the crystalline form of agomelatine V for the treatment of sexual dysfunctions, as an ovulation inhibitor, immunomodulator in the treatment of cancer.

Kristalni V oblik agomelatina, biće pre svega korišćen za lečenje opšte depresije, sezonskih depresija, poremećaja spavanja, kardiovaskularnih patologija, patologija digestivnog sistema, nesanica i umora kao posledica vremenske razlike, poremećaja apetita i gojaznosti. The crystalline V form of agomelatine will primarily be used for the treatment of general depression, seasonal depression, sleep disorders, cardiovascular pathologies, digestive system pathologies, insomnia and fatigue as a result of time difference, appetite disorders and obesity.

Pronalazak se, isto tako, odnosi na farmaceutske smeše koje kao aktivni princip sadrže kristalni V oblik jedinjenja formule (I) sa jednom ili više inertnih podloga, koje su netoksične i koje su odgovarajuće. Od farmaceutskih smeša koje su u skladu sa pronalaskom, mogu se naročito navesti one koje su pogodne za primenjivanje oralnim putem, parenteralnim (intravenskim ili subkutanim), nazalnim putem, kao jednostavne pilule ili dražeje, granule, sublingvalne pilule, želatinske kapsule, tablete, supozitorije, kremovi, masti, gelovi za kožu, injektabilni preparati, suspenzije za oralnu upotrebu i gume za žvakanje. The invention also relates to pharmaceutical mixtures which as active principle contain the crystalline V form of the compound of formula (I) with one or more inert bases, which are non-toxic and which are appropriate. Of the pharmaceutical mixtures according to the invention, those suitable for oral, parenteral (intravenous or subcutaneous), nasal administration, such as simple pills or dragees, granules, sublingual pills, gelatin capsules, tablets, suppositories, creams, ointments, skin gels, injectable preparations, suspensions for oral use and chewing gums, can be mentioned in particular.

Doziranje koje će biti delotvorno se podešava prema prirodi i težini bolesti, načinu primenjivanja, kao i starosti i težini pacijenta. Ovakvo doziranje varira od 0,1 mg do 1 g na dan u jednoj ili više doza. The dosage that will be effective is adjusted according to the nature and severity of the disease, the method of administration, as well as the age and weight of the patient. This dosage varies from 0.1 mg to 1 g per day in one or more doses.

Primeri u nastavku ilustruju pronalazak, ali ga ni na koji način ne ograničavaju. The following examples illustrate the invention, but do not limit it in any way.

Primer 1:Kristalni V oblik A/-[2-(7-metoksi-1-naftil)etil]acetamidaExample 1: Crystalline form V of A/-[2-(7-methoxy-1-naphthyl)ethyl]acetamide

100 g A/-[2-(7-metoksi-1-naftil)etil]acetamida je stavljeno u mehanički mlin tipa varioplanetarnog mlina u toku otprilike 6 sati i dobijena čvrsta masa je opisana pomoću dijagrama difrakcije X zraka na dobijenom prašku, što je mereno na difraktometru Siemens D5005 (bakarna antikatoda) i izraženo kao među-mrežna udaljenost d, ugao Bragg 2 teta i, relativni intenzitet (izražen u procentima u odnosu na najintenzivniju prugu): 100 g of A/-[2-(7-methoxy-1-naphthyl)ethyl]acetamide was placed in a mechanical mill of the varioplanetary mill type for approximately 6 hours and the resulting solid mass was described by X-ray diffraction pattern of the obtained powder, which was measured on a Siemens D5005 diffractometer (copper anticathode) and expressed as interlattice distance d, Bragg angle 2 theta i, relative intensity (expressed in percentages compared to the most intense streak):

Primer 2: Kristalni V oblik A/-[2-(7-metoksi-1-naftil)etil]acetamidaExample 2: Crystalline form V of N-[2-(7-methoxy-1-naphthyl)ethyl]acetamide

4 g de /V-[2-(7-metoksi-1-naftil)etil]acetamida je stavljeno u ventilirani sušionik na 110°C. Posle sat vremena na 110°C, proizvod je ohlađen do temperature sredine i zasejan sa 0,05 g kristalnog V oblika A/-[2-(7-metoksi-1-naftil)etil]acetamida koji strukturno čist i koji je dobijen pomoću visoko energetskog mlina. Posle 5 minuta, kristalizacija je završena i dobijena čvrsta masa je opisana pomoću dijagrama difrakcije X zraka na dobijenom prašku, što je mereno na difraktometru Siemens D5005 (bakarna antikatoda) i izraženo kao među-mrežna udaljenost d, ugao Bragg 2 teta i, relativni intenzitet (izražen u procentima u odnosu na najintenzivniju prugu): 4 g of N-[2-(7-methoxy-1-naphthyl)ethyl]acetamide was placed in a ventilated dryer at 110°C. After one hour at 110° C., the product was cooled to ambient temperature and seeded with 0.05 g of structurally pure crystalline form V of A/-[2-(7-methoxy-1-naphthyl)ethyl]acetamide obtained using a high energy mill. After 5 minutes, the crystallization is complete and the resulting solid is described by X-ray diffraction pattern of the obtained powder, which was measured on a Siemens D5005 diffractometer (copper anticathode) and expressed as inter-lattice distance d, Bragg angle 2 theta i, relative intensity (expressed as a percentage of the most intense line):

Primer 3: Farmaceutska smešaExample 3: Pharmaceutical composition

Formula za izradu 1000 tableta u dozi od po 25 mg : Formula for making 1000 tablets in a dose of 25 mg each:

Primer 4:Farmaceutska smešaFormula za izradu 1000 tableta u dozi od po 25 mg : Example 4: Pharmaceutical mixture Formula for making 1000 tablets in a dose of 25 mg each:

Claims (2)

1. Kristalni oblik V agomelatina formule (I): naznačen time štoje dijagram difrakcije X zraka na dobijenom prašku kako sledi, a što je mereno na difraktometru Siemens D5005 (bakarna antikatoda) i izraženo kao među-mrežna udaljenost d, ugao Bragg 2 teta i, relativni intenzitet (izražen u procentima u odnosu na najintenzivniju prugu): 1. Crystal form V agomelatine of formula (I): indicated by the X-ray diffraction pattern on the resulting powder as follows, which was measured on a Siemens D5005 diffractometer (copper anticathode) and expressed as inter-lattice distance d, Bragg angle 2 theta i, relative intensity (expressed as a percentage of the most intense line): 2. Postupak za proizvodnju kristalnog V oblika jedinjenja formule (I), prema zahtevu 1,naznačen time štose agomelatin podvrgava mehaničkom mlevenju u visoko energetskom mlinu.2. The method for the production of the crystalline V form of the compound of formula (I), according to claim 1, characterized by subjecting agomelatine to mechanical grinding in a high-energy mill.
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