関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 5-Acetoxy-4,6-di-tert-butylbenzofuran | HCID 11822332 | — |
| 生成物 | 5-Acetoxy-4,6-di-tert-butyl-2-formylbenzofuran | HCID 22918669 | 86% |
反応手順
Phosphorus oxychloride (1.1 g) was added dropwise to N,N-dimethylformamide (0.4 g) under cooling with ice and, subsequently, a solution of 5-acetoxy-4,6-di-tert-butylbenzofuran (1.0 g) in N,N-dimethylformamide (2 ml) was added dropwise. The mixture was stirred first at room temperature for 20 min, then under heating at 80° C. for 75 min. After cooling, the reaction mixture was poured into water and subjected to extraction 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-formylbenzofuran [0.95 g (yield, 86%)] as a colorless, fine-grained crystal.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05574178 |
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| 出典データセット | uspto-grants-1996_11 |
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| ORD ID | ord-c88de32d11294de09695eac5ba48c948 |
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| 出典メモ | uspto-grants-1996_11 |
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