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Chloroacetyl chloride → 6-Chloro-nicotinic Acid N'-(2-chloro-acetyl)-hydrazide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroacetyl chloride | HCID 6577 | — |
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | 6-Chloropyridine-3-carbohydrazide | HCID 2800177 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 6-Chloro-nicotinic Acid N'-(2-chloro-acetyl)-hydrazide | HCID 58997462 | 57% |
反応手順
Chloroacetyl chloride (2.8 mL, 34.9 mmol) was added dropwise to an ice-cooled solution of 6-chloronicotinic acid hydrazide (5 g, 29.1 mmol) and 4-methylmorpholine (4.8 mL, 43.7 mmol) in dichloromethane (100 mL) and the reaction was stirred at room temperature for 3 hours. The resulting precipitate was then filtered off, slurried with dichloromethane, re-filtered, washed with dichloromethane (×3) and dried to afford the title compound as a beige solid in 57% yield, 4.1 g
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07649003B2 |
| 出典データセット | uspto-grants-2010_01 |
| ORD ID | ord-982cef7ee92c457faa692f7d8bc32aa5 |
| 出典メモ | uspto-grants-2010_01 |