関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cyanoacetamide | HCID 7898 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 2-Fluoro-5-nitroaniline | HCID 67785 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(2-Amino-4-nitrophenyl)-2-cyanoacetamide | HCID 59189936 | 94% |
反応手順
Potassium tert-butoxide (36 g, 0.32 mol) was added to a solution of 2-cyanoacetamide (27 g, 0.32 mol) in anhydrous N,N-dimethylformamide (700 mL), and a solution of 2-fluoro-5-nitroaniline (25 g, 0.16 mol) in anhydrous N,N-dimethylformamide (80 mL) was added dropwise thereto under ice-cooling. After the reaction mixture was stirred at 5° C. for 18 hours, it was poured into a saturated ammonium chloride aqueous solution (1.0 L) under ice-cooling. The whole was extracted with ethyl acetate (1.0 L). The organic layer was washed with water (500 mL), brine (300 mL), and dried over anhydrous magnesium sulfate. After the solvent was evaporated under reduced pressure, toluene (100 mL) and dichloromethane (100 mL) were added to the residue. The precipitated solid was filtered off, and dried under reduced pressure to give the title reference compound (33 g) as a brown solid (yield 94%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08193237B2 |
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| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-953f7f56d69d4386834a259c4141091a |
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| 出典メモ | uspto-grants-2012_06 |
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