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HRID 131456作成日:2026年10月27日

Dimethyl Sulfoxide → (S)-7-Chloro-10-[3-(3-methoxy-propyl)-piperazin-1-yl]-4H-3-thia-4,9-diaza-benzo[f]azulene

https://huagongshe.com/reaction/131456

反応式

関与物質

役割名称HCID仕込み量
反応物Dimethyl SulfoxideHCID 679—
反応物TolueneHCID 1140—
反応物(2S)-2-(3-Methoxypropyl)piperazineHCID 45099475—
反応物7-Chloro-4H-3-thia-4,9-diaza-benzo[f]azulen-10-ylamine hydrochlorideHCID 136388576—
溶媒Ethyl AcetateHCID 8857—
生成物(S)-7-Chloro-10-[3-(3-methoxy-propyl)-piperazin-1-yl]-4H-3-thia-4,9-diaza-benzo[f]azuleneHCID 13609041226.1%

反応条件

温度105 °C

反応手順

Combine 7-chloro-4H-3-thia-4,9-diaza-benzo[f]azulen-10-ylamine hydrochloride (786.7 mg, 2.75 mmol), (S)-2-(3-methoxy-propyl)-piperazine (870.0 mg, 5.50 mmol), DMSO (2.0 ml), and toluene (8.0 ml). Stir and heat the mixture at 105° C. After 48 hours, cool the mixture to ambient temperature. Dilute the mixture with ethyl acetate and wash the organic layer with 0.1N NaOH and brine. Dry (sodium sulfate) and concentrate the organic layer to residue. Purify the residue on silica gel using a gradient of dichloromethane to dichloromethane/methanol (90:10) to give 280.3 mg (26%) of the title compound: mass spectrum (ion spray): m/z=391.1 (M+1).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07384934B2
出典データセットuspto-grants-2008_06
ORD IDord-7bd72c75277b47248d9caddc669b5009
出典メモuspto-grants-2008_06