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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

反応式

関与物質

役割名称HCID仕込み量
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]azuleneHCID 57900185—
溶媒PyridineHCID 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]azuleneHCID 5820380640.2%

反応条件

温度160 °C

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US08673952B2
出典データセットuspto-grants-2014_03
ORD IDord-52af37fe387e43d8b700a673a037423d
出典メモuspto-grants-2014_03