化工社化工社 化学情報印刷レポート · 研究参考用
Dichloromethane → (Z)-3-(3-nitro-4-methoxyphenyl)-2-(3,4,5-trimethoxyphenyl)-prop-2-ene-nitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 3,4,5-Trimethoxyphenylacetonitrile | HCID 25887 | — |
| 反応物 | 4-Methoxy-3-nitrobenzaldehyde | HCID 700608 | — |
| 触媒 | N-Methyloctan-1-amine--hydrogen chloride (1/1) | HCID 22561414 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (Z)-3-(3-nitro-4-methoxyphenyl)-2-(3,4,5-trimethoxyphenyl)-prop-2-ene-nitrile | HCID 10619131 | 72.4% |
反応手順
3.0 g of 3-nitro-4-methoxybenzaldehyde, 3.4 g of 3,4,5-trimethoxyphenylacetonitrile, 800 mg of sodium hydroxide and 100 mg of octylmethylammonium chloride were dissolved in 15 ml of water and 15 ml of dichloromethane and reacted for 4 hours at room temperature. Ice water was added to the reaction liquid, which was then extracted three times each with dichloromethane. The extract was dried with anhydrous sodium sulfate and concentrated. The concentrated liquid was purified by crystallization (ethyl acetate) to obtain 4.4 g of the intended compound. The yield was 72%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05525632 |
| 出典データセット | uspto-grants-1996_06 |
| ORD ID | ord-1fc0a5e64cea4a7692a615b3c55a2b09 |
| 出典メモ | uspto-grants-1996_06 |