化工社化工社 化学情報印刷レポート · 研究参考用
1,3-Diethyl 2-oxopropanedioate → Diethyl 2-(2-methyl-2-propionylhydrazono)malonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,3-Diethyl 2-oxopropanedioate | HCID 69105 | — |
| 反応物 | N-methylpropionohydrazide | HCID 542680 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Diethyl 2-(2-methyl-2-propionylhydrazono)malonate | HCID 57442166 | 49% |
反応手順
A solution of N-methylpropionohydrazide (18.78 g, 183.9 mmol) and diethyl ketomalonate (56.1 mL, 368 mmol) in toluene (136 mL) was refluxed with a Dean-Stark trap for 4 hours. The reaction mixture was concentrated under reduced pressure to give the crude material that was purified by silica gel flash column chromatography (100% hexanes to 5 to 10% EtOAc in hexanes) to afford 23 g (49%) of the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07732616B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-5cdca83ee7f64971b5c07200968b6b9d |
| 出典メモ | uspto-grants-2010_06 |