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HRID 375276作成日:2026年10月25日

Water → N-tert-butyl-2-(3-azido-2-oxo-5-phenyl-2,3,4,5-tetrahydro-1H-(1)benzazepin-1-yl) ethanoic acid amide

https://huagongshe.com/reaction/375276

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物DimethylformamideHCID 6228—
反応物Sodium AzideHCID 33557—
反応物N-tert-butyl 2-(3-bromo-2-oxo-5-phenyl-2,3,4,5-tetrahydro-1H-(1)benzazepin-1-yl) ethanoic acid amideHCID 15203361—
溶媒Ethyl AcetateHCID 8857—
生成物N-tert-butyl-2-(3-azido-2-oxo-5-phenyl-2,3,4,5-tetrahydro-1H-(1)benzazepin-1-yl) ethanoic acid amideHCID 15203363—

反応条件

温度75 °C

反応手順

To a 250 ml round-bottomed flask equipped with N2 inlet were added N-tert-butyl-2-[3-bromo-2-oxo-5-phenyl-2,3,4,5-tetrahydro-1H-(1)benzazepin-1-yl] ethanoic acid amide, (8.317 g, 19.37 mmoles), 90 ml dimethylformamide (DMF), and sodium azide (5.25 g, 80 mmoles, under nitrogen), and the mixture was heated at 75° C. for 20 hours with stirring. The reaction mixture was then cooled and distributed between water and ethyl acetate, separated, and the aqueous phase was again extracted. The combined extracts were washed with water three times, with bicarbonate solution once, and then dried with brine and sodium sulfate and filtered and evaporated, leaving a gummy residue, 8.58 g (100%), containing some solvent.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05484917
出典データセットuspto-grants-1996_01
ORD IDord-0f850b766acd4aac878515543dd33df7
出典メモuspto-grants-1996_01