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HRID 71144作成日:2026年10月26日

Sodium hydride → Ethyl 3-(3,4-difluorobenzyl)-2-oxopiperidine-3-carboxylate

https://huagongshe.com/reaction/71144

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium hydrideHCID 24758—
反応物3-Carbethoxy-2-piperidoneHCID 97773—
反応物4-(Bromomethyl)-1,2-difluorobenzeneHCID 581436—
溶媒DimethylformamideHCID 6228—
溶媒Ethyl AcetateHCID 8857—
溶媒Ammonium ChlorideHCID 25517—
生成物Ethyl 3-(3,4-difluorobenzyl)-2-oxopiperidine-3-carboxylateHCID 66607767—

反応条件

温度0 °C

反応手順

Under a nitrogen atmosphere, to a mixture of ethyl 2-oxopiperidine-3-carboxylate (2.0 g) in DMF (20 mL) was added sodium hydride (60%, 0.47 g) at 0° C., and the mixture was stirred at 0° C. for 30 min. 4-(Bromomethyl)-1,2-difluorobenzene (1.50 mL) was added to the reaction mixture, and the mixture was stirred at room temperature overnight. The reaction mixture was diluted with ethyl acetate and saturated aqueous ammonium chloride solution, the mixture was washed with saturated brine and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (2.82 g).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08822699B2
出典データセットuspto-grants-2014_09
ORD IDord-6984390e460d42cfaf5e95d0ceef91d0
出典メモuspto-grants-2014_09