関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Phenoxyphenol | HCID 12842 | — |
| 反応物 | Tin tetrachloride | HCID 24287 | — |
| 反応物 | Triethyl methanetricarboxylate | HCID 80471 | — |
| 生成物 | 4-Hydroxy-2-oxo-7-phenoxy-2H-chromene-3-carboxylic acid ethyl ester | HCID 86649463 | 4.5% |
反応手順
A mixture of 3-phenoxy-phenol (1.068 g, 5.73 mmol), 2-ethoxycarbonyl-malonic acid diethyl ester (3.65 mL, 17.2 mmol), and tin tetrachloride (14 μL, 0.11 mmol) was heated in a 200° C.-oil bath for 5 min; then cooled, the reaction mixture was directly purified on silica gel column chromatography (eluent: ethyl acetate in dichloromethane: 10% to 80%) to give the desired title product (84 mg, 4.4%). ESI (m/z): 327 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08324405B2 |
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| 出典データセット | uspto-grants-2012_12 |
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| ORD ID | ord-f55ba2a4ea184d8a9cbba303f3198f6d |
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| 出典メモ | uspto-grants-2012_12 |
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