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HRID 657554作成日:2026年10月27日

Hydrochloric Acid → 7,8-dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepine hydrochloride

https://huagongshe.com/reaction/657554

反応式

関与物質

役割名称HCID仕込み量
反応物Hydrochloric AcidHCID 313—
反応物EthanolHCID 702—
反応物Borane;tetrahydrofuranHCID 2723981—
反応物7,8-dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepin-2-oneHCID 11401769—
溶媒TetrahydrofuranHCID 8028—
生成物7,8-dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepine hydrochlorideHCID 22004098—

反応条件

温度0 °C

反応手順

22.13 g (100 mmol) of the product obtained in Step 1, suspended in 250 mL of THF, are cooled to 0° C. There are then added, dropwise, over 15 minutes, 250 mL of borane/THF (1M in the THF) and heating is carried out at 80° C. for 24 hours. Cooling is carried out and there are then added, dropwise, 250 mL of ethanol, and then 2.6N ethanolic HCl. Heating at reflux is carried out for 40 minutes; some light insoluble material is filtered off and evaporation to dryness is carried out. The residue thereby obtained is recrystallised from a mixture of 150 mL of isopropanol and 20 mL of water to yield the desired product.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08076325B2
出典データセットuspto-grants-2011_12
ORD IDord-36f8f94c5ab04e7ea8422c96ea1e1876
出典メモuspto-grants-2011_12