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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
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | (2S)-2-(3-Methoxypropyl)piperazine | HCID 45099475 | — |
| 反応物 | 7-Chloro-4H-3-thia-4,9-diaza-benzo[f]azulen-10-ylamine hydrochloride | HCID 136388576 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | (S)-7-Chloro-10-[3-(3-methoxy-propyl)-piperazin-1-yl]-4H-3-thia-4,9-diaza-benzo[f]azulene | HCID 136090412 | 26.1% |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07384934B2 |
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| 出典データセット | uspto-grants-2008_06 |
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| ORD ID | ord-7bd72c75277b47248d9caddc669b5009 |
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| 出典メモ | uspto-grants-2008_06 |
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