化工社化工社 化学情報印刷レポート · 研究参考用
tert-Butylhydrazine monohydrochloride → 6-(4-Chlorophenyl)-4,5-dihydro-2-t-butylpyridazinone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | tert-Butylhydrazine monohydrochloride | HCID 81889 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 4-Chlorobenzoylpropionic acid | HCID 18917115 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | 6-(4-Chlorophenyl)-4,5-dihydro-2-t-butylpyridazinone | HCID 18917116 | 34.4% |
反応手順
To a solution of 4-chlorobenzoylpropionic acid (4.24 g) in n-butanol (150 ml) was added anhydrous sodium acetate (1.54 g) and t-butylhydrazine hydrochloride (2.75 g) portionwise at room temperature. The resulting mixture was refluxed for 9 hours distilling off 65 ml of n-butanol during that time. The resulting mixture was cooled and poured into water (500 ml) and extracted with methylene chloride (3×150 ml). The combined organic layers were washed with 2% aqueous sodium hydroxide (3×100 ml), water (2×100 ml), 2% aqueous hydrochloric acid (3×100 ml), and water (1×100 ml), dried and evaporated under vacuum yielding 1.71 g of the expected product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05728698 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-01437a3fcaad437da9c411fa39cdbc01 |
| 出典メモ | uspto-grants-1998_03 |