化工社化工社 化学情報印刷レポート · 研究参考用
1-(3,4-Dimethylphenyl)hydrazine hydrochloride → 4-[(3-bromo-2-methoxyphenyl)hydrazinylidene]-2-(3,4-dimethylphenyl)-5-methylpyrazol-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-(3,4-Dimethylphenyl)hydrazine hydrochloride | HCID 173740 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | HCID 178472845 | HCID 178472845 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 4-[(3-bromo-2-methoxyphenyl)hydrazinylidene]-2-(3,4-dimethylphenyl)-5-methylpyrazol-3-one | HCID 178486378 | — |
反応手順
A solution of ethyl-2-[(3-bromo-2-methoxyphenyl)hydrazono]-3-oxobutanoate (5 g) prepared as in Example 1, and 3,4-dimethylphenylhydrazine hydrochloride (2.48 g) and sodium acetate (1.4 g) in glacial acetic acid (100 mL) was stirred and heated to reflux for about 3 hours. The mixture was cooled to about room temperature and stirred for about 1 hour. It was filtered, washed with water (25 mL) and dried in an oven at about 55° C. to about 60° C. for about 12 hours to obtain an orange solid product. Yield: 4.15 g; Melting point: 197.4-198.2° C.; Purity (HPLC): 99.33%
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09440927B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-82ebaf342c6448da820299c8ce483664 |
| 出典メモ | uspto-grants-2016_09 |