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HRID 15727作成日:2026年10月25日

Triethylamine → 4-chloro-N-(1-diazo-2-oxopentan-3-yl)-N-(pent-1-yn-3-yl)benzenesulfonamide

https://huagongshe.com/reaction/15727

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物DiazomethaneHCID 9550—
反応物Isobutyl chloroformateHCID 62365—
反応物2-(4-chloro-N-(pent-1-yn-3-yl)phenylsulfonamido)-butanoic acidHCID 59342373—
溶媒Acetic AcidHCID 176—
溶媒Diethyl EtherHCID 3283—
生成物4-chloro-N-(1-diazo-2-oxopentan-3-yl)-N-(pent-1-yn-3-yl)benzenesulfonamideHCID 72259587—

反応条件

温度-30 °C

反応手順

To a solution of the compound 60 (498 mg, 1.45 mmol) in 7.5 mL of Et2O were added sequentially 0.24 mL of triethylamine (1.2 eq), 0.23 mL of isobutyl chloroformate (1.2 eq) at −30° C. After being stirred at −30° C. for 15 min, diazomethane (prepared by mixing MNNG and KOH in diethyl ether) (excess) was added to the above mixture at 0° C. and stirred there for 5 hours. Glacial HOAc (1.5 mL) was added to destroy the excess diazomethane and the solution was extracted with EtOAc. The organic phase was washed with sat NaHCO3, water, brine and dried (MgSO4). LCMS 368.1 (M+1).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07732609B2
出典データセットuspto-grants-2010_06
ORD IDord-c6a04bb7504c4ce18d8cc8e65ca5dd39
出典メモuspto-grants-2010_06