PROCESS FOR PRODUCING 1-/3-CHLORO-PHENYL/-4-METHYL-7,8-DIMETHOXY-5H-2,3-BENZODIAZEPINE OF HIGH PURITY

• Main Authors: BALOGH,TIBOR,HU, ORBAN,ERNOE,HU, GYENGE,ROZSA,HU, BOTKA,PETER,HU, SOMOGYI,GYOERGY,HU, KOEROESI,JENOE,HU, KISS,CSILLA,HU, HORVATH,GYULA,HU, HAMORI,TAMAS,HU, USKERT,ANDORNE,HU, SIMAY,ANTAL,HU, BIDLO,GABORNE,HU, MORAVCSIK,IMRE,HU
• Format: Patent
• Language: English
• Published: 28.10.1993
• Edition: 5
• Subjects: CHEMISTRY; HETEROCYCLIC COMPOUNDS; HUMAN NECESSITIES; HYGIENE; MEDICAL OR VETERINARY SCIENCE; METALLURGY; ORGANIC CHEMISTRY; PREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES; SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS ORMEDICINAL PREPARATIONS

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.