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-Benzyloxy-4-t-butylbenzofuran | HCID 23442878 | — |
| 生成物 | 5-Benzyloxy-4-t-butyl-2-formylbenzofuran | HCID 23442879 | 36% |
反応手順
Phosphorus oxychloride (26.2 ml, 0.29 mol) was added dropwise to N,N-dimethylformamide (17 ml, 0.22 mol) under ice cooling; subsequently, a solution of 5-benzyloxy-4-tert-butylbenzofuran (40 g, 0.14 mol) in N,N-dimethylformamide (10 ml) was added dropwise. The mixture was stirred first at room temperature for 20 min, then under heating at 80° C. for 2 h. After cooling, the reaction mixture was poured into water and extracted with ethyl acetate. The extracted layer was washed with a saturated aqueous solution of sodium hydrogen carbonate and water, dried over anhydrous magnesium sulfate and concentrated. The concentrate was purified by silica gel chromatography (10% ethyl acetate in n-hexane) to afford 5-benzyloxy-4-tert-butyl-2-formylbenzofuran [16.2 g (yield, 36%)].
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-64b81a10165f407bb58ab61a8212e312 |
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| 出典メモ | uspto-grants-1997_09 |
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