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4-Methylmorpholine → N-methoxy-N-methyl-2-methyl-6-trifluoromethyl-3-pyridinecarboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 2-Methyl-6-(trifluoromethyl)nicotinic acid | HCID 2775683 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-methoxy-N-methyl-2-methyl-6-trifluoromethyl-3-pyridinecarboxamide | HCID 86625530 | — |
反応手順
To a solution of 2-methyl-6-trifluoromethylnicotinic acid (500 mg, 2.44 mmol) and N,O-dimethylhydroxylamine hydrochloride (285 mg, 2.92 mmol) in dichloromethane (10 mL) were added N-methylmorpholine (0.32 mL, 2.92 mmol) and N-(3-dimethylaminopropyl-N′-ethylcarbodiimide hydrochloride (EDC, 560 mg, 2.92 mmol). The mixture was stirred at room temperature for 2 hours and washed with 1 N HCl and water. The organic layer was dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure to give N-methoxy-N-methyl-2-methyl-6-trifluoromethyl-3-pyridinecarboxamide quantitatively as oil. The crude product was used directly in the following reaction.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07858621B2 |
| 出典データセット | uspto-grants-2010_12 |
| ORD ID | ord-1b95cf3a764647c0823983b8e57c2aa7 |
| 出典メモ | uspto-grants-2010_12 |