関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Malonic Acid | HCID 867 | — |
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | 4-Methoxy-3-nitrobenzaldehyde | HCID 700608 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 3-{3-Nitro-4-methoxyphenyl}acrylic acid | HCID 821746 | — |
反応手順
4-methoxy-3-nitro-benzaldehyde (compound of Example 5; 1.05 g, 5.79 mmol) and malonic acid (1.32 g, 1.27 mmol) were dissolved in pyridine (20 mL) under stirring and piperidine (1 mL) was added to the pyridine solution. The reaction mixture was heated at 75° C. to 80° C. for 3 h, after which the temperature was further increased to 120° C. and maintained at this temperature for 6 h. At the end of the reaction, pyridine was evaporated, followed by addition of aqueous HCl (1:1) to obtain pH ˜4. The solid obtained was filtered, washed with cold water and dried.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08629277B2 |
|---|
| 出典データセット | uspto-grants-2014_01 |
|---|
| ORD ID | ord-c9716e3dc2f346b3bd78114fc4c8aab5 |
|---|
| 出典メモ | uspto-grants-2014_01 |
|---|