化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 2-Propenoic acid, 3-(2-chloro-4-fluorophenyl)-
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 | 2-Chloro-4-fluorobenzaldehyde | HCID 145024 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 2-Propenoic acid, 3-(2-chloro-4-fluorophenyl)- | HCID 2725065 | 96% |
反応手順
To a mixture of 2-chloro-4-fluorobenzaldehyde (20.0 g, 0.13 mol, Aldrich) and malonic acid (26.2 g, 0.25 mol, Aldrich) in pyridine (100 ml) at 50° C. was added dropwise piperidine (10 ml). After 18 h at 70° C., the mixture was poured into an ice cold solution of concentrated HCl (120 ml) and water (1.5 L). The resulting solid was filtered and washed repeatedly with water to give 24.4 g (96%) of 2-chloro-4-fluoro-cinnamic acid as a white solid: Recrystallization of 1.5 g from acetone:water mixtures gave 1.1 g of 2-chloro-4-fluorocinnamic acid as a white solid: mp 243°-245° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05708033 |
| 出典データセット | uspto-grants-1998_01 |
| ORD ID | ord-7b250f591ac24bd79e4f5435df536049 |
| 出典メモ | uspto-grants-1998_01 |