関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Methoxyphenol | HCID 9007 | — |
| 反応物 | 3-Fluorophenylacetic acid | HCID 67617 | — |
| 生成物 | 2-(3-Fluorophenyl)-1-(2-hydroxy-4-methoxyphenyl)ethanone | HCID 17978504 | — |
反応手順
(3-Fluorophenyl)acetic acid (3.7 g) and 3-methoxyphenol (3.0 g) were dissolved into BF3Et2O (60 ml, 20 eq) under argon. The mixture was stirred at 60-70° C. until disappearance of the starting materials (9 h) and poured into large volume of ice water. After extraction with ethyl acetate the combined organic layers were washed with water, dried and evaporated. The crude product was purified by column chromatography using CH2Cl2 as an eluant. 1H NMR (400 MHz, d6-DMSO) δ: 12.41 (br s, 1H), 8.02 (d, 1H, J 9.0 Hz), 7.34-7.38 (m, 1H), 7.09-7.13 (m, 3H), 6.56 (dd, 1H, J 9.0, 2.5 Hz), 6.49 (d, 1H, J 2.5 Hz), 4.41 (s, 2H), 3.83 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07425568B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-1391c4fde4464f7eb0e82249779eb5ee |
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| 出典メモ | uspto-grants-2008_09 |
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