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HRID 587059作成日:2026年10月25日

Water → Methyl 7-[4-(2-butoxyethoxy)phenyl]-1-(2-butynyl)-2,3-dihydro-1-benzazepine-4-carboxylate

https://huagongshe.com/reaction/587059

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Sodium hydrideHCID 24758—
反応物1-Bromo-2-butyneHCID 2756862—
反応物methyl 7-[4-(2-butoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylateHCID 22328987—
溶媒TetrahydrofuranHCID 8028—
生成物Methyl 7-[4-(2-butoxyethoxy)phenyl]-1-(2-butynyl)-2,3-dihydro-1-benzazepine-4-carboxylateHCID 22328992—

反応手順

In THF (24.0 ml) was dissolved methyl 7-[4-(2-butoxyethoxy)phenyl]-2,3-dihydro-1-benzazepine-4-carboxylate (1.20 g). To the solution was added 60% sodium hydride (0.24 g), and the mixture was stirred at room temperature for 1 hour. To the mixture was added 1-bromo-2-butyne (0.80 ml), and the mixture was stirred at 65° C. for 4 days. After cooled to room temperature, the reaction solution was added to water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine and dried with magnesium sulfate. The solvent was removed under reduced pressure, and the resulting residue was purified with silica gel column chromatography (hexane/ethyl acetate=4/1) to give methyl 7-[4-(2-butoxyethoxy)phenyl]-1-(2-butynyl)-2,3-dihydro-1-benzazepine-4-carboxylate (0.50 g).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06936602B1
出典データセットuspto-grants-2005_08
ORD IDord-74f01aa5068e4d44be7b05c6d1542084
出典メモuspto-grants-2005_08