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HRID 57745作成日:2026年10月23日

Hydrochloric Acid → Diethyl 2-benzyloxycarbonylamino-2-(benzyloxycarbonylmethyl)malonate

https://huagongshe.com/ja/reaction/57745

反応式

関与物質

役割名称HCID仕込み量
反応物Hydrochloric AcidHCID 313—
反応物Sodium hydrideHCID 24758—
反応物Benzyl bromoacetateHCID 62576—
反応物Diethyl 2-(benzyloxycarbonylamino)malonateHCID 259787—
溶媒DimethylformamideHCID 6228—
生成物Diethyl 2-benzyloxycarbonylamino-2-(benzyloxycarbonylmethyl)malonateHCID 6672516399%

反応手順

A solution of diethyl 2-benzyloxycarbonylaminomalonate (30 g) in anhydrous DMF (100 mL) was added portionwise with sodium hydride (60%, 4.27 g) with ice cooling and stirring, then the mixture was stirred at room temperature for 30 minutes, and then added with benzyl 2-bromoacetate (28.9 g), and the mixture was stirred overnight. The reaction mixture was poured into diluted hydrochloric acid, the mixture was extracted with ethyl acetate, and the extract was washed with saturated brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was subjected to silica gel column chromatography, and then purification was performed with n-hexane/ethyl acetate (4:1), to obtain the title compound (43.9 g, yield: 99%) as colorless oil.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09434737B2
出典データセットuspto-grants-2016_09
ORD IDord-602dde33759e487e961a51b22824aeaa
出典メモuspto-grants-2016_09