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Morpholine → (6-Aminopyridin-3-yl)(morpholino)methanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | 6-Aminonicotinic acid | HCID 18496 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | (6-Aminopyridin-3-yl)(morpholino)methanone | HCID 59259223 | 34.3% |
反応手順
To a solution of morpholine (9.00 g, 103 mmol) in 400 mL ethanol was added N-(3-Dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (10.0 g, 52.2 mmol), 1-hydroxybenzotriazole (7.00 g, 51.8 mmol), and 6-aminonicotinic acid (6.00 g, 43.4 mmol). After stirring for 18 hours, the resulting solid was filtered. This was triturated with a mixture of 100 mL methanol and 100 mL dichloromethane to yield (6-Amino-pyridin-3-yl)-morpholin-4-yl-methanone (3.08 g, 14.9 mmol). MS (ESI) 208.1 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822457B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-333f6a181a9a4c4b8df2a3415efa8db1 |
| 出典メモ | uspto-grants-2014_09 |