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HRID 3676作成日:2026年10月23日

Sulfuric Acid → (S)-7-[(1,3-Dihydro-1,3-dioxo-2H-isoindol-2-yl)]-1,2,6,7,8,12b-hexahydro-6-oxopyrido[2,1-a][2]benzazepine

https://huagongshe.com/ja/reaction/3676

反応式

関与物質

役割名称HCID仕込み量
反応物Sulfuric AcidHCID 1118—
反応物Trifluoroacetic anhydrideHCID 9845—
反応物Sodium BicarbonateHCID 516892—
反応物(S)-N-[2-(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)-1-oxo-3-phenylpropyl]-1,4-dihydro-pyridineHCID 15380836—
溶媒Ethyl acetate hexaneHCID 21226206—
生成物(S)-7-[(1,3-Dihydro-1,3-dioxo-2H-isoindol-2-yl)]-1,2,6,7,8,12b-hexahydro-6-oxopyrido[2,1-a][2]benzazepineHCID 9863597—

反応手順

Combine sulfuric acid (3.0 mL, 96%) and trifluoroacetic anhydride (300 mL). Add (S)-N-[2-(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)-1-oxo-3-phenylpropyl]-1,4-dihydro-pyridine (1.0 mmol). After 30 minutes, pour the reaction mixture into a mixture of saturated aqueous sodium bicarbonate and ice. Extract with ethyl acetate and then with methylene chloride. Combine the organic layers and filter through a plug of silica gel. Rinse the silica gel with dichloromethane. Evaporate the filtrate in vacuo to give a residue. Chromatograph the residue on silica gel eluting sequentially with 10% ethyl acetate/hexane and then 25% ethyl acetate/hexane to give the title compound.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05734049
出典データセットuspto-grants-1998_03
ORD IDord-f3c835216c0344d1af2af2f75940e898
出典メモuspto-grants-1998_03