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HRID 8749作成日:2026年10月23日

Lithium Hydroxide → Tert-butyl 1-oxo-8-azaspiro(4.5)decane-8-carboxylate

https://huagongshe.com/ja/reaction/8749

反応式

関与物質

役割名称HCID仕込み量
反応物Lithium HydroxideHCID 3939—
反応物8-tert-Butyl 2-methyl 1-oxo-8-azaspiro[4.5]decane-2,8-dicarboxylateHCID 21983897—
溶媒Ethanol tetrahydrofuran waterHCID 18504229—
生成物Tert-butyl 1-oxo-8-azaspiro(4.5)decane-8-carboxylateHCID 1084848767.5%

反応条件

温度90 °C

反応手順

To a solution of tert-butyl 2-(methoxycarbonyl)-1-oxo-8-azaspiro[4.5]decane-8-carboxylate (17.2 g, 0.055 mol) from Step F in a 2:2:1 mixture of ethanol/tetrahydrofuran/water (555 mL) was added pulverized lithium hydroxide (26 g, 1.10 mol). The reaction mixture was heated to 90° C. for 60 h. The reaction mixture was allowed to cool and was then concentrated, dissolved in water and dichloromethane, and extracted three times with dichloromethane. The organic layers were combined, washed with brine, dried over sodium sulfate, filtered, and concentrated to afford 11.4 g. The residue was purified by flash chromatography eluting with 20–30% ethyl acetate in hexanes to give the title compound (9.41 g).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07091211B2
出典データセットuspto-grants-2006_08
ORD IDord-279bb325608143949a9c5045f8750794
出典メモuspto-grants-2006_08