関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-(2-aminoethyl)acetamide | HCID 66082 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2,6-Dichloro-3-nitropyridine | HCID 85239 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-(2-(6-chloro-3-nitropyridin-2-ylamino)ethyl)acetamide | HCID 43553026 | — |
反応手順
To a solution of 3.0 g (15.5 mmol) 2,6-dichloro-3-nitropyridine in 50 mL of THF at −78° C. under Ar atmosphere was added 2.7 mL (15.5 mmol) of N,N-diisopropylethylamine followed by 1.6 mL (15.5 mmol) of N-acetylethylenediamine. The mixture was stirred at −78° C. for 30 min, allowed to warm to room temperature, and stirred for 72 hours. The solvent was removed in vacuo and the residue was purified by flash chromatography eluting with MeOH/dichloromethane gradient (1→10%) to provide N-(2-(6-chloro-3-nitropyridin-2-ylamino)ethyl)acetamide as pale yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07732453B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-6afd05ca531e403db75e62f03c7e5b13 |
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| 出典メモ | uspto-grants-2010_06 |
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