化工社化工社 化学情報印刷レポート · 研究参考用
Pyridine → 3,5-Dimethyl-1-phenyl-1H-pyrazole-4-carboxylic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Phenylhydrazine | HCID 7516 | — |
| 反応物 | Ethyl 2-acetylacetoacetate | HCID 79063 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3,5-Dimethyl-1-phenyl-1H-pyrazole-4-carboxylic acid ethyl ester | HCID 656964 | — |
反応手順
Similar to Example 1, phenyl hydrazine (7.5 mmol, 0.8 g) and 2-acetyl-3-oxo-butyric acid ethyl ester (7.5 mmol, 1.3 g) were mixed in a solution of 50% pyridine in ethanol. The solvents were removed under vacuum and the oil resuspended in chloroform. The resulting suspension was washed with 5% sodium bicarbonate, 5% hydrochloric acid, and then brine. The organic layer was dried over NaSO4, the solids filtered, and the solvents removed under vacuum. The crude material was purified over silica gel to yield the named product as an oil. 1H-NMR (CDCl3, ppm): 1.37 t (3H); 2.51 s (6H); 4.32 q (2H); 7.42 bs (5H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07087634B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-32740fb7cd88475c80964fc430e15578 |
| 出典メモ | uspto-grants-2006_08 |