化工社化工社 化学情報印刷レポート · 研究参考用
Diethyl (ethoxymethylene)malonate → HCID 178418871、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl (ethoxymethylene)malonate | HCID 6871 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Methyl-2-thiopseudourea sulfate | HCID 75270 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 178418871 | HCID 178418871 | 61% |
反応手順
To a 4N sodium hydroxide solution (200 mL) was added S-methylisothioureasulfate (55.6 g, 0.2 mol), and after stirring for 30 min, at room temperature a solution of diethyl ethoxymethylenemalonate (80.8 mL, 0.35 mol) in ethanol (100 mL) was dropwise added slowly over 1 h. After stirring for 18 h, the precipitated crystals were collected by filtration, washed several times with cold ethanol and the obtained crystals were added to 1N hydrochloric acid (300 mL). The mixture was stirred for 30 min and the precipitated crystals were collected by filtration, washed several times with cold water and dried with heating under vacuum to give the title compound (26 g, 61%) as crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07087597B1 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-347b46abced84de9bf8ce6a178260fd5 |
| 出典メモ | uspto-grants-2006_08 |