関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Chloronicotinonitrile | HCID 81079 | — |
| 反応物 | 2,4-Dimethoxybenzylamine | HCID 597250 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | 2-(2,4-Dimethoxybenzylamino)nicotinonitrile | HCID 22293175 | 72.2% |
反応手順
2,4-Dimethoxybenzylamine (2.90 g, 17.3 mmol) and triethylamine (1.75 g, 17.3 mmol) were added sequentially to a solution of 2-chloronicotinonitrile (2.0 g, 14.4 mmol) in N,N-dimethylacetamide (29 mL). The reaction was heated at 80° C. for 4 h, quenched with water and extracted with diethyl ether (3×). The combined organic extracts were washed water, saturated brine, dried over magnesium sulfate and concentrated. The crude product was purified by flash chromatography (silica gel, 0-5% ethyl acetate (with 0.1 triethylamine) in dichloromethane gradient elution) to produce the title compound (2.80 g). MS 270.3 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07745427B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-8d936463582b49538798f5c256ddebf8 |
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| 出典メモ | uspto-grants-2010_06 |
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