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4-Methylmorpholine → 6-Chloro-nicotinic Acid N'-[2-(2-methoxy-ethoxy)-acetyl]-hydrazide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 6-Chloropyridine-3-carbohydrazide | HCID 2800177 | — |
| 反応物 | 2-(2-Methoxyethoxy)acetyl chloride | HCID 7010338 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 6-Chloro-nicotinic Acid N'-[2-(2-methoxy-ethoxy)-acetyl]-hydrazide | HCID 58997430 | 51% |
反応手順
(2-Methoxy-ethoxy)-acetyl chloride (2.13 g, 13.99 mmol) was added to an ice-cold solution of 6-chloronicotinic acid hydrazide (2 g, 11.66 mmol) and N-methylmorpholine (1.92 mL, 17.49 mmol) in dichloromethane (60 mL) and the mixture was stirred at room temperature for 18 hours. The mixture was then treated with sodium hydrogen carbonate solution and concentrated in vacuo. The aqueous residue was extracted with dichloromethane (×2) and the combined organic solutions were washed with brine and dried over sodium sulfate and concentrated in vacuo to give a pale yellow residue. The residue was then stirred in diethyl ether for 2 hours, filtered and dried to afford the title compound as a pale yellow solid in 51% yield, 1.7 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07875615B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-3d8be728137444bebfe65289ba627e72 |
| 出典メモ | uspto-grants-2011_01 |