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HRID 394843作成日:2026年10月25日

Triethylamine → Ethyl 1,4-dibenzylpiperazine-2-carboxylate

https://huagongshe.com/reaction/394843

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物BenzathineHCID 8793—
反応物Ethyl 2,3-dibromopropionateHCID 97945—
溶媒TolueneHCID 1140—
生成物Ethyl 1,4-dibenzylpiperazine-2-carboxylateHCID 2736402—

反応条件

温度80 °C

反応手順

To a stirred solution of ethyl 2,3-dibromopropionate (142.7 g, 0.549 mol) in dry toluene (2000 mL) was added N,N′-dibenzylethylene diamine (132 g, 0.549 mol), followed by triethylamine (110.8 g, 1.098 mol), under N2 at 40° C. (a dense white precipitate formed immediately, thus good stirring was necessary). The mixture was heated at 80° C. overnight, cooled and filtered. The filtrate was then washed with H2O, dried over MgSO4, and concentrated under reduced pressure. The residue oil was taken on to the next step without further purification (GC-MS shows one peak at 6.79) or purified by column chromatography (EtOAc/hexane 1:4). Weight of crude product: 169.6 g (91%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06603002B2
出典データセットuspto-grants-2003_08
ORD IDord-2e3192318cb6481abc502dea0f2d66af
出典メモuspto-grants-2003_08