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Ethyl trifluoroacetate → 4,4,4-Trifluoro-1-(pyridin-2-yl)butane-1,3-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl trifluoroacetate | HCID 9794 | — |
| 反応物 | 2-Acetylpyridine | HCID 14286 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4,4,4-Trifluoro-1-(pyridin-2-yl)butane-1,3-dione | HCID 2771478 | 81.2% |
反応手順
Trifluoro-acetic acid ethyl ester (9.82 mL, 82.5 mmol) was added to a solution of 1-pyridin-2-yl-ethanone (5.00 g, 41.2 mmol) in methanol (40 mL) containing sodium methoxide (61.8 mmol). The reaction mixture was heated at reflux overnight, concentrated under reduced pressure and acidified with aqueous hydrochloric acid (10%). The aqueous solution was extracted with ethyl acetate (10×50 mL). The organic layers were collected, dried over sodium sulfate, filtered, and concentrated under reduced pressure. The crude product was purified by column chromatography on silica gel to give 4,4,4-trifluoro-1-pyridin-2-yl-butane-1,3-dione (7.26 g, 81%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07098335B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-041f2cc851b84257b82bcd81cc91efb6 |
| 出典メモ | uspto-grants-2006_08 |