関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3,5-Dimethylisoxazole | HCID 9312 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Methyl 2-tert.butyldimethylsiloxybenzoate | HCID 131719984 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 2-(3-Methyl-isoxazol-5-yl)-1-(2-tert.butyldimethylsiloxy-phenyl)-ethanone | HCID 131719983 | 50.4% |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05622953 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-a7602e0c89e6449eacff8936f61394cd |
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| 出典メモ | uspto-grants-1997_04 |
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