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HRID 64726作成日:2026年10月26日

Ethyl Acetate → 16beta-Ethyl-17beta-(3-oxobutyryl)oxyacetoxy-4-estren-3-one

https://huagongshe.com/reaction/64726

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DiketeneHCID 12661—
反応物Sodium AcetateHCID 517045—
反応物16beta-Ethyl-17beta-glycoloyloxy-4-estren-3-oneHCID 70466441—
溶媒DichloromethaneHCID 6344—
生成物16beta-Ethyl-17beta-(3-oxobutyryl)oxyacetoxy-4-estren-3-oneHCID 70467327—

反応手順

In 30 ml of dichloromethane is dissolved 0.8 g of 16β-ethyl-17β-glycoloyloxy-4-estren-3-one, and 0.24 g of anhydrous sodium acetate and 0.3 ml of diketene are added. The mixture is refluxed for 4 hours. After cooling, 100 ml of ethyl acetate is added and the mixture is washed with water and saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate. The solvent is then distilled off under reduced pressure and the residue is subjected to column chromatography. Following serial passage of 400 ml of diisopropyl ether and 400 ml of diisopropyl ether-ethyl acetate (10:1), elution is carried out with 600 ml of isopropyl ether-ethyl acetate (2:3). The eluate is evaporated under reduced pressure to remove the solvent, giving 1.0 g of the above-identified compound as a light-yellow viscous oil.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04609650
出典データセットuspto-grants-1986_09
ORD IDord-a12a091f133c40afb685201a87e3a710
出典メモuspto-grants-1986_09