関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Heptyltriphenylphosphonium bromide | HCID 2724567 | — |
| 反応物 | 5-Acetoxy-4,6-di-tert-butyl-2-formylbenzofuran | HCID 22918669 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Pentane | HCID 8003 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-Acetoxy-4,6-di-tert-butyl-2-(1-octenyl)benzofuran | HCID 53768721 | 97% |
反応手順
A pentane solution (6.0 ml) of 1.6M n-butyllithium was added dropwise to a solution of n-heptyltriphenylphosphonium bromide (4.2 g) in tetrahydrofuran (30 ml) under a nitrogen atmosphere. After stirring the mixture at room temperature for 90 min, a solution of 5-acetoxy-4,6-di-tert-butyl-2-formylbenzofuran (2.54 g) in tetrahydrofuran (20 ml) was added dropwise. Subsequently, the mixture was heated under reflux for 1 h and, after cooling, a saturated aqueous solution of ammonium chloride was added and the mixture was subjected to extraction with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate and concentrated. The concentrate was purified by silica gel chromatography (10% ethyl acetate in n-hexane) to afford 5-acetoxy-4,6-di-tert-butyl-2-(1-octenyl)benzofuran [3.1 g (yield, 97%)] as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05663373 |
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| 出典データセット | uspto-grants-1997_09 |
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| ORD ID | ord-1dddc5be3d3f4f748a456c8ab929c8b9 |
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| 出典メモ | uspto-grants-1997_09 |
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