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HRID 5729作成日:2026年10月24日

Dimethylformamide → Benzyl 1,4-diazepane-1-carboxylate

https://huagongshe.com/ja/reaction/5729

反応式

関与物質

役割名称HCID仕込み量
反応物DimethylformamideHCID 6228—
反応物Benzyl chloroformateHCID 10387—
反応物Hexahydro-1,4-diazepineHCID 68163—
反応物Sodium BicarbonateHCID 516892—
溶媒WaterHCID 962—
生成物Benzyl 1,4-diazepane-1-carboxylateHCID 438495565.5%

反応手順

To 230 ml of dimethylformamide were added 25 g of homopiperazine and 5.4 g of sodium bicarbonate and then 25 ml of water followed by dropwise addition of 10 g of benzyloxycarbonyl chloride with stirring under ice cooling, and the mixture was stirred at a room temperature overnight. After evaporating off dimethylformamide under a reduced pressure, the reaction mixture was extracted three times with 100 ml of chloroform, and the extract was dried over magnesium sulfate and evaporated to remove the solvent under a reduced pressure. The resulting residue was applied to a silica gel column and eluted with chloroform/methanol (9:1), to obtain 9 g of the title compound as a light yellow liquor liquid.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05245034
出典データセットuspto-grants-1993_09
ORD IDord-9210acb815974a8380d54b730e8abe69
出典メモuspto-grants-1993_09