関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,3-Dinitrophenol | HCID 6191 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | tert-Butyl bromoacetate | HCID 79177 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Ethyl 2-(2,3-dinitrophenoxy)acetate | HCID 86642030 | 70% |
反応手順
A round-bottom flask was charged with 2,3-dinitrophenol (11.04 g, 60 mmol, commercially available from Fluka-Sigma-Aldrich), tert-butyl bromoacetate (14.05 g, 66 mmol), acetonitrile (120 mL) and cesium carbonate (21.6 g). The mixture was stirred at room temperature overnight. The mixture was filtered, and the recovered solid was washed with ethyl acetate. The filtrate was further diluted with ethyl acetate and water. The aqueous layer was extracted with ethyl acetate and combined organic solvent was washed with saturated brine, dried and concentrated under reduced pressure. The residue was triturated with ether to give ethyl 2-(2,3-dinitrophenoxy)acetate (13.0 g, 70% yield). 1H-NMR (DMSO-d6) δ 7.84 (d, 2H), 7.42 (s, 1H), 4.90 (s, 2H), 1.40 (S, 9H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08088767B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-b12faa9f3aab45d38b7a14f8b7d45680 |
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| 出典メモ | uspto-grants-2012_01 |
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