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-Fluoro-2-methylbenzaldehyde | HCID 2783217 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 4-Fluoro-2-methylcinnamic acid | HCID 54775776 | 69% |
反応手順
A stirred solution of 4-fluoro-2-methyl-benzaldehyde (20 g, 144.9 mmol) and malonic acid (30.1 g, 289.8 mmol) in pyridine (100 mL) was heated to 50° C. Piperidine (10 mL) was added and the reaction mixture was heated at 70° C. for 18 h. The reaction mixture was cooled RT and poured into chilled aqueous 1N HCl solution (1500 mL), the resulting precipitate was filtered and washed with petroleum ether 60-80 and dried in vacuo to obtain (E)-3-(4-fluoro-2-methylphenyl)acrylic acid (18 g, 69%) as an off white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09193689B2 |
|---|
| 出典データセット | uspto-grants-2015_11 |
|---|
| ORD ID | ord-8f856b60844c4a909a0cce1f822c5b95 |
|---|
| 出典メモ | uspto-grants-2015_11 |
|---|
