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HRID 58384作成日:2026年10月25日

Ethyl Acetate → (7S,10S,13S)-10-Isopropyl-13-methanesulfonylamino-9,12-dioxo-2-oxa-8,11-diaza-bicyclo[13.2.2]nonadeca-1(18),15(19),16-triene-7-carboxylic acid methyl ester

https://huagongshe.com/reaction/58384

反応式

関与物質

役割名称HCID仕込み量
反応物Ethyl AcetateHCID 8857—
反応物Methanesulfonyl chlorideHCID 31297—
反応物DiisopropylethylamineHCID 81531—
反応物(7S,10S,13S)-13-Amino-10-isopropyl-9,12-dioxo-2-oxa-8,11-diaza-bicyclo[13.2.2]nonadeca-1-(18),15(19),16-triene-7-carboxylic acid methyl ester hydrogen chloride saltHCID 86650244—
溶媒DimethylformamideHCID 6228—
生成物(7S,10S,13S)-10-Isopropyl-13-methanesulfonylamino-9,12-dioxo-2-oxa-8,11-diaza-bicyclo[13.2.2]nonadeca-1(18),15(19),16-triene-7-carboxylic acid methyl esterHCID 66847432—

反応手順

Amine 47 (200 mg) was dissolved in anhydrous DMF (5 mL). Methane-sulfonyl chloride (39 μL) and DIPEA (0.175 mL) were added and the reaction mixture was stirred at rt for 18 h before being partitioned between chloroform and 1M hydrochloric acid. The aqueous phase was extracted three more times with chloroform and the combined organic extracts were dried (MgSO4), filtered and concentrated in vacuo. Purification was achieved using flash chromatography, eluting with a gradient of 1/1 EtOAc/(50/70) petroleum ether to EtOAc to yield a light brown solid, 40 mg, 17%. Rf=0.12 (1/1 EtOAc/(50/70) petroleum ether).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09434762B2
出典データセットuspto-grants-2016_09
ORD IDord-575659e4f17d478492d17ddc7a65ed3b
出典メモuspto-grants-2016_09