化工社化工社 化学情報印刷レポート · 研究参考用
Water → HCID 9857126、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1,3-Dichloroacetone | HCID 10793 | — |
| 反応物 | 4-(Trifluoromethyl)cinnamamide | HCID 5709014 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 9857126 | HCID 9857126 | 63.1% |
反応手順
A mixture of (E)-3-(4-trifluoromethylphenyl)-2-propenamide (17.9 g) and 1,3-dichloroacetone (14.8 g) in toluene (83 ml) was refluxed for 9 hours by use of Dean-Stark apparatus. After cooling, the reaction mixture was combined with water, extracted with ethyl acetate, washed with saturated brine, and dried over magnesium sulfate, then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane:ethyl acetate=6:1 to 5:1) to give the titled compound (15.1 g) as colorless needle crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06984653B2 |
| 出典データセット | uspto-grants-2006_01 |
| ORD ID | ord-f5e6a1b5218143e3a243ec9ba534379d |
| 出典メモ | uspto-grants-2006_01 |