関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cyanoacetamide | HCID 7898 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-(2-Chlorophenyl)-2-(4-chlorophenyl)-3-(dimethylamino)prop-2-en-1-one | HCID 68658840 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-(2-Chlorophenyl)-5-(4-chlorophenyl)-2-oxo-1,2-dihydropyridine-3-carbonitrile | HCID 21984907 | — |
反応手順
A solution of the crude product from step A dissolved in 80 mL of DMF containing 4.4 mL methanol and 4.61 g cyanoacetamide was transferred by cannula into a flask containing a suspension of NaH (4.98 g, 60% dispersion in mineral oil, freed of excess oil by washing with hexane just prior to use) in DMF (40 mL). The solution was heated to 95° C. for 2.5 hours then concentrated. The residue was dissolved in ethyl acetate, washed twice with 10% aqueous NaHSO4, and twice with water before concentrating to a solid. The solid was suspended in warm ethanol and then cooled, and the title compound was subsequently isolated by filtration and dried in vacuo.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07091216B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-a4bf6cda5e1b41fbb814ac2110f72af8 |
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| 出典メモ | uspto-grants-2006_08 |
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