化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 4-Allyloxy-3-nitrocinnamic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Malonic Acid | HCID 867 | — |
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | 4-Allyloxy-3-nitrobenzaldehyde | HCID 22401152 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 4-Allyloxy-3-nitrocinnamic acid | HCID 54381117 | 70.3% |
反応手順
4-Allyloxy-3-nitrobenzaldehyde (5 g, 24.1 mM) was dissolved in pyridine (100 ml) and malonic acid (5.02 g, 48.3 mM) and piperidine (0.48 ml, 4.8 mM) added. The mixture was heated to reflux with stirring for 2 hours, cooled, and poured onto a mixture of concentrated hydrochloric acid and ice. Organics were extracted into ethyl acetate, the organic layer washed with 2M hydrochloric acid, and product back-extracted into aqueous NaHCO3. The aqueous solution was then re-acidified (concentrated hydrochloric acid), and organics extracted into ethyl acetate, washed with brine, and dried (MgSO4), to give title compound (4.23 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05527791 |
| 出典データセット | uspto-grants-1996_06 |
| ORD ID | ord-2d00ecb238134095b6b0426401ec41a6 |
| 出典メモ | uspto-grants-1996_06 |