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Hydrochloric Acid → 6-chloro-N'-{6-[methyl(phenyl)amino]pyridazin-3-yl}pyridine-2-carbohydrazide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 6-Chloropicolinic acid | HCID 20812 | — |
| 反応物 | 6-hydrazino-N-methyl-N-phenylpyridazine-3-amine | HCID 21081844 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 6-chloro-N'-{6-[methyl(phenyl)amino]pyridazin-3-yl}pyridine-2-carbohydrazide | HCID 21081843 | 30.5% |
反応手順
To a solution of 6-hydrazino-N-methyl-N-phenylpyridazine-3-amine (1.14 g) in methylene chloride (10 ml), 6-chloropicolic acid (0.83 g) and WSCD hydrochloride (1.22 g) were added, and the mixture was stirred at room temperature overnight. The reaction solution was purified by silica gel column chromatography (eluent: chloroform) to obtain 6-chloro-N′-{6-[methyl(phenyl)amino]pyridazin-3-yl}pyridine-2-carbohydrazide (0.57 g). This compound (0.56 g) was stirred at 150° C. overnight in xylene (20 ml), and the reaction solution was concentrated to obtain 3-(chloropyridin-2-yl)-N-methyl-N-phenyl-1,2,4-triazolo[4,3-b]pyridazine-6-amine (0.54 g) as colorless solids.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07173033B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-0d15d04f87134a0ea1bdf49eb3d5b4f2 |
| 出典メモ | uspto-grants-2007_02 |