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HRID 4033作成日:2026年10月23日

4-Bromo-6-(4-methyl-1-piperazinyl)-9-methyl-1,2-dihydrobenzo[b]-pyrrolo [3,2,1-jk][1,4]benzodiazepine → 4-Bromo-6-(4-methyl-1-piperazinyl)-9-methylbenzo[b]pyrrolo-[3,2,1-jk][1,4]benzodiazepine

https://huagongshe.com/ja/reaction/4033

反応式

関与物質

役割名称HCID仕込み量
反応物4-Bromo-6-(4-methyl-1-piperazinyl)-9-methyl-1,2-dihydrobenzo[b]-pyrrolo [3,2,1-jk][1,4]benzodiazepineHCID 13823314—
触媒HCID 178418406HCID 178418406—
溶媒ChloroformHCID 6212—
生成物4-Bromo-6-(4-methyl-1-piperazinyl)-9-methylbenzo[b]pyrrolo-[3,2,1-jk][1,4]benzodiazepineHCID 1382330842.7%

反応手順

To a solution of 4-bromo-6-(4-methyl-1-piperazinyl)-9-methyl-1,2-dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepine (5.7 g, 13.8 mmoles) in chloroform (540 ml) was added manganese dioxide (25 gm), and the mixture was heated under reflux for 4 days. The mixture was filtered, and the filter cake washed with dichloromethane. The filtrate was concentrated under vacuum. The residue was purified on a silica gel column, eluted with 2% methanol/dichloromethane. The fractions (75-100 ml each) containing pure product were pooled and concentrated. Recrystallization from a small volume of 2-propanol yielded 2.41 g (42%) of product, mp 153°-155° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04723007
出典データセットuspto-grants-1988_02
ORD IDord-9d63ac06d4b64e4ca99b120a96de594c
出典メモuspto-grants-1988_02