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HRID 36697作成日:2026年10月24日

N-methylhydroxylamine hydrochloride → Ethyl 2,4-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

https://huagongshe.com/ja/reaction/36697

反応式

関与物質

役割名称HCID仕込み量
反応物N-methylhydroxylamine hydrochlorideHCID 77906—
反応物Sodium AcetateHCID 517045—
反応物ethyl N-(but-2-enyl)-N-(2-oxoethyl)-carbamateHCID 53690408—
溶媒WaterHCID 962—
溶媒1,4-DioxaneHCID 31275—
生成物Ethyl 2,4-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylateHCID 15070019—

反応手順

18.4 g (0.1 mol) of ethyl N-(but-2-enyl)-N-(2-oxoethyl)-carbamate are dissolved in 100 ml of dioxane, and 9 g of anhydrous sodium acetate and 9 g (0.108 mol) of N-methylhydroxylamine hydrochloride in 10 ml of water are added. The mixture is heated under reflux overnight and cooled and the salts are filtered off with suction and washed with dioxane. The filtrate is concentrated, the residue is taken up in 100 ml of water and K2CO3 is added. The mixture is extracted with CHCl3, the extract is dried over K2CO3 and concentrated and the residue is distilled.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05416096
出典データセットuspto-grants-1995_05
ORD IDord-c363c3f6a8394ce3b9913ed620fe0370
出典メモuspto-grants-1995_05