化工社化工社 化学情報印刷レポート · 研究参考用
Ethyl Acetoacetate → Ethyl 2-acetyl-3-methyl-4-oxopentanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetoacetate | HCID 8868 | — |
| 反応物 | 2-Butanone, 3-bromo- | HCID 13142 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 2-acetyl-3-methyl-4-oxopentanoate | HCID 14689360 | — |
反応手順
7.3 G., 0.317 mol of sodium was dissolved in 125 ml. of absolute ethanol 87.0 G. (0.669 mol) of ethyl acetoacetate were added to the resulting solution of sodium ethoxide in the cold. The reaction mixture was heated to reflux and 48.6 g. (0.322 mol) of freshly distilled 3-bromo-2-butanone were added dropwise with stirring over a period of 30 min. Refluxing was continued until the mixture tested neutral to pH paper (~1.5 hrs.). The precipitated sodium bromide was filtered off the cold solution and most of the ethanol was removed on an evaporator. The mixture was filtered again and distilled. The 3-ethoxycarbonyl-4-methyl-hexane-2,4-dione fraction which boiled at 131°-137° C./18 mm. was collected.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04256878 |
| 出典データセット | uspto-grants-1981_03 |
| ORD ID | ord-e4e4ce6b926d4505b8a6a5bfaade3f85 |
| 出典メモ | uspto-grants-1981_03 |