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HRID 43936作成日:2026年10月25日

Water → HCID 68406269、化合物

https://huagongshe.com/reaction/43936

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-IodopropaneHCID 33643—
反応物Benzyl 4-((tert-butoxycarbonyl)amino)piperidine-1-carboxylateHCID 21981786—
溶媒TetrahydrofuranHCID 8028—
生成物HCID 68406269HCID 6840626926.7%

反応手順

A solution of benzyl 4-[(tert-butoxycarbonyl)amino]piperidine-1-carboxylate obtained in Example (241a) (1.00 g, 2.99 mmol) in THF (5 mL) was added to a suspension of sodium hydride (55%) (261 mg, 5.98 mmol) in THF (25 mL) at 0° C. Subsequently, propyl iodide (1.46 mL, 15.0 mmol) was added at 0° C., and the mixture was stirred at room temperature for 22 hours. Thereafter, sodium hydride (55%) (130 mg, 2.99 mmol) and propyl iodide (0.58 mL, 5.98 mmol) were added, and the mixture was heated under reflux for 22 hours. Water was added to the reaction solution, and the mixture was extracted with ethyl acetate. Thereafter, the combined organic layers were washed with brine and dried over anhydrous magnesium sulfate. Following filtration, the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=5/1) to obtain 301 mg of the title compound as a pale yellow oily substance (27%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08536197B2
出典データセットuspto-grants-2013_09
ORD IDord-62988030973a43508cfc013c231c063f
出典メモuspto-grants-2013_09