POSTUPAK ZA DOBIJANJE 1-(3-HLOROFENIL)-4-METIL-7,8-DIMETOKSI-5H-2,3-BENZODIAZEPINA VELIKE ČISTOĆE

POSTUPAK ZA DOBIJANJE 1-(3-HLOROFENIL)-4-METIL-7,8-DIMETOKSI-5H-2,3-BENZODIAZEPINA VELIKE ČISTOĆE, pronalazak se odnosi na postupak za dobijanje 1-(3-hlorofenil)-4-mestil-7,8-dimetoksi-5-h-2,3-benzodiazepina formule (I) velike čistoće i kvaliteta podesnih za farmaceutske potrebe. Prema pronalasku reakcija 1 mola 2-acetonil-3'-hloro-4,5-dimetoksi-fenona formule (II) sa 3-7 mola hidrazin hidrata u organskom rastvaraču ili u smeši organskih rastvarača na temperaturi izmedju 15В°C i 85В°C vrši se u odsustvu kiseonika iz vazduha, opcionalno u prisustvu vode. Sirovi proizvod se zatim rekristališe iz alifatičnog alkohola koji sadrži 1 do 5 atoma ugljenika. Pronalazak se takodje odnosi na postupak za prečišćavanje 1-(3-hlorofenil)-4-metil-7,8-dimetoksi-5H-2,3-ben-zodiazepina formule (I). 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.