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HRID 1190271作成日:2026年10月26日
2-Propanamine, hydrochloride (1:1) → 8-Bromo-2-(4-isopropyl-4H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene
https://huagongshe.com/reaction/1190271
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
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| 反応物 | 2-Propanamine, hydrochloride (1:1) | HCID 6432137 | — |
| 反応物 | 8-Bromo-2-[1,3,4]oxadiazol-2-yl-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene | HCID 57900185 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 8-Bromo-2-(4-isopropyl-4H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene | HCID 58203806 | 40.2% |
反応手順
To a solution of 8-bromo-2-[1,3,4]oxadiazol-2-yl-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene (4.38 g, 12.51 mmol) in pyridine (12 mL) was added isopropylamine hydrochloride (1.38 g, 12.51 mmol). The reaction mixture was heated at 160° C. for 30 minutes using microwave irradiation before being concentrated in vacuo. The residue was taken up into DCM then washed with 1M HCl then brine before being dried (Na2SO4) and concentrated in vacuo. The resultant residue was purified by flash chromatography (SiO2, gradient 0-3% methanol in DCM then further purified, gradient 0-4% MeOH in EtOAc) to yield the title compound as an orange solid (1.97 g, 40%). LCMS: RT=4.67 min, M+H+=391/393.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08673952B2 |
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| 出典データセット | uspto-grants-2014_03 |
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| ORD ID | ord-52af37fe387e43d8b700a673a037423d |
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| 出典メモ | uspto-grants-2014_03 |
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