VERFAHREN ZUR HERSTELLUNG VON 1-(3'-(CHLORO)- PHENYL>-4-(METHYL>-7,8-DI-(METHOXY>-5H-2,3- BENZODIAZEPIN HOHER REINHEIT

According to an aspect of the invention there is provided for a process for the preparation of 1-[3'-(chloro)-phenyl]-4-[methyl[-7,8-di-[methoxy]-5H-2,3-benzodiazepine of formula in high purity and in a quality suitable for pharmaceutical purposes by reacting 1 mole of 2-(acetonyl)-3'-(chl...

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Hauptverfasser: ORBAN, ERNOE, BOTKA, PETER, KOEROESI, JENO, GYENGE, ROZSA, HAMORI, TAMAS, HORVATH, GYULA, BALOGH, TIBOR, SIMAY, ANTAL, KISS, CSILLA, BIDLO NEE IGLOI, MARIA, MORAVCSIK, IMRE, USKERT NEE DIEVALD, EMILIA, SOMOGYI, GYOERGY
Format: Patent
Sprache:ger
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Zusammenfassung:According to an aspect of the invention there is provided for a process for the preparation of 1-[3'-(chloro)-phenyl]-4-[methyl[-7,8-di-[methoxy]-5H-2,3-benzodiazepine of formula in high purity and in a quality suitable for pharmaceutical purposes by reacting 1 mole of 2-(acetonyl)-3'-(chloro)-4,5-di-(methoxy)-benzophenone of formula with 3 to 7 moles of hydrazine hydrate in an organic solvent or in a mixture of organic solvents, at a temperature from 15 DEG C to 85 DEG C, and subsequently recrystallizing the crude product from an aliphatic alcohol containing 1 to 5 carbon atom(s), which is carried out in the absence of air oxygen. According to another aspect of the invention there is provided for a process for preparing purified 1-[3'-(chloro)-phenyl]-4-[methyl]-7,8-di-[methoxy]-5H-2,3-benzodiazepine of formula I from such containing contamination(s) of formula and/or particularly formula in which first the contaminated 1-[3'-(chloro)-phenyl]-4-[methyl]-7,8-di-[methoxy]-5H-2,3-benzodiazepine of formula I is treated with a solvent and an alkali hydroxide, alkali carbonate or alkali alcoholate and thereafter the compound 1-[3'-(chloro)-phenyl]-4-[methyl]-7,8-di-[methoxy]-5H-2,3-benzodiazepine of formula I is crystallized from the obtained solution.