化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → alpha-Methyl-4-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 | Methylmalonic Acid | HCID 487 | — |
| 反応物 | 4-Nitrobenzaldehyde | HCID 541 | — |
| 反応物 | Piperidine | HCID 8082 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | alpha-Methyl-4-nitrocinnamic acid | HCID 235115 | — |
反応手順
630 ml of pyridine was added to 76 g of 4-nitrobenzaldehyde (m.p. 105°-106.5° C.), 118 g of methylmalonic acid (prepared by hydrolysis of diethyl methylmalonate) and 85 g of piperidine. The mixture was heated with stirring over a steam bath for 24 hours. After being allowed to cool, the reaction mixture was then added to a mixture of 1,250 ml of concentrated hydrochloric acid and 2.5 kg of ice. The resulting oil content was then extracted with diethyl ether. The oil content was further extracted with a 5% aqueous solution of sodium hydroxide. The aqueous solution was then slightly acidified. The resulting crystal composition was then filtered off and dried. (Yield: 86 g (83%))
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04994363 |
| 出典データセット | uspto-grants-1991_02 |
| ORD ID | ord-15d003794798414d8244bb38881d6034 |
| 出典メモ | uspto-grants-1991_02 |