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HRID 1389184作成日:2026年10月27日

Hexane → Ethyl 5-Hydroxy-4-methyl-7-(1-methyl-4-phenylbutyl)coumarin-3-propionate

https://huagongshe.com/reaction/1389184

反応式

関与物質

役割名称HCID仕込み量
反応物HexaneHCID 8058—
反応物Phosphorus oxychlorideHCID 24813—
反応物Diethyl 2-acetylglutarateHCID 73915—
反応物5-(5-Phenylpentan-2-yl)benzene-1,3-diolHCID 20487367—
溶媒ChloroformHCID 6212—
生成物Ethyl 5-Hydroxy-4-methyl-7-(1-methyl-4-phenylbutyl)coumarin-3-propionateHCID 53719146—

反応手順

A mixture of 2-(3,5-dihydroxyphenyl)-5-phenylpentane (33 g., 0.13 M), (Preparation C) diethyl α-acetoglutarate (32.2 g., 0.14 M) and phosphorous oxychloride (20 g., 0.13 M), protected from atmospheric moisture, is stirred at room temperature. After 10 days, the mixture is dissolved in chloroform, washed three times with water, dried (Na2SO4), and evaporated. The residue is subjected to silica gel chromatography (eluents--9 benzene:1 ether) to yield 22 g. of the desired ester, m.p. 58°-70° C. from hexane. Further recrystallization from ethyl acetate/hexane affords an analytical sample: m.p. 78°-85° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04243674
出典データセットuspto-grants-1981_01
ORD IDord-0decae391ec24e7f9a84a79f28035cc6
出典メモuspto-grants-1981_01