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Ethanol → Diethyl 2-nitro-4-benzoylphenylmalonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Diethyl Malonate | HCID 7761 | — |
| 反応物 | 4-Chloro-3-nitrobenzophenone | HCID 41743 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Diethyl 2-nitro-4-benzoylphenylmalonate | HCID 13408230 | — |
反応手順
To a solution of sodium ethoxide, formed by reacting 4.6 g. (0.2 mole) of sodium metal with 200 ml. of ethanol, at 0° C. was added 32 g. (0.2 mole) of diethyl malonate followed by 26.1 g. (0.1 mole) of 4-chloro-3-nitrobenzophenone. The mixture was allowed to stir at room temperature for 2 hours and was then poured into 400 ml. of ice cold 2N hydrochloric acid and 300 ml. of methylene chloride. The organic layer was separated, dried over magnesium sulfate and concentrated to an oil. The residual oil was induced to crystallize by trituration with hexane containing trace amounts of diisopropyl ether, 34.75 g., m.p. 68°-70° C. The sample was further purified by trituration with hot hexane-diisopropyl ether, 30.84 g. (80% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04725616 |
| 出典データセット | uspto-grants-1988_02 |
| ORD ID | ord-c0dad1d0d168495ea764fd1fd6e209c1 |
| 出典メモ | uspto-grants-1988_02 |