関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexamethylphosphoramide | HCID 12679 | — |
| 反応物 | 4-iodo-N-methyl-3-nitrobenzamide | HCID 20755545 | — |
| 生成物 | N-methyl-4-cyano-3-nitrobenzamide | HCID 57331535 | 55.2% |
反応手順
2 g (6.53 mmol) N-methyl-4-iodo-3-nitrobenzamide (Compound VII-1), 0.09 g (10.0 mmol) cuprous cyanide and 10 ml hexamethylphosphoric triamide were added into a reaction flask. The mixture was heated to 100° C. and reacted for 40 minutes, and after completing the reaction, the mixture was cooled to room temperature, and then extracted with ethyl acetate. The organic layer was washed with water for three times, dried over anhydrous sodium sulfate, decolorized with activated charcoal, filtered, and the filtrate was concentrated to dryness, recrystallized from ethyl acetate to obtain 0.74 g N-methyl-4-cyano-3-nitrobenzamide (Compound I-27), yield 55.2%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08946478B2 |
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| 出典データセット | uspto-grants-2015_02 |
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| ORD ID | ord-2883e507c52c425595d2a93084f6f789 |
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| 出典メモ | uspto-grants-2015_02 |
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