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HRID 54421作成日:2026年10月24日

3,5-Dimethylisoxazole → 2-(3-Methyl-isoxazol-5-yl)-1-(2-tert.butyldimethylsiloxy-phenyl)-ethanone

https://huagongshe.com/ja/reaction/54421

反応式

関与物質

役割名称HCID仕込み量
反応物3,5-DimethylisoxazoleHCID 9312—
反応物Ammonium ChlorideHCID 25517—
反応物Methyl 2-tert.butyldimethylsiloxybenzoateHCID 131719984—
反応物ButyllithiumHCID 178418339—
溶媒TetrahydrofuranHCID 8028—
溶媒HexaneHCID 8058—
生成物2-(3-Methyl-isoxazol-5-yl)-1-(2-tert.butyldimethylsiloxy-phenyl)-ethanoneHCID 13171998350.4%

反応条件

温度-20 °C

反応手順

52 ml of 1N solution of n-butyllithium in hexane were added to a solution of 6 g of 3,5-dimethylisoxazol in 200 ml of tetrahydrofuran at -78° C. After stirring for 1 h 15 g of methyl 2-tert.butyldimethylsiloxybenzoate in 50 ml of tetrahydrofuran were added at the same temperature. The reaction mixture was slowly warmed up to -20° C. A saturated aqueous solution of ammonium chloride was added, the mixture was extracted several times with ethylacetate. The organic phase was separated, washed with water and dried over magnesium sulfate. Chromatography on silica gel with heptane/ethylacetate gave 9.4 g of the product.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05622953
出典データセットuspto-grants-1997_04
ORD IDord-a7602e0c89e6449eacff8936f61394cd
出典メモuspto-grants-1997_04