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4-Pyridinecarboxylic acid, 1-oxide → N-[4-chloro-3-(trifluoromethyl)phenyl]-4-pyridinecarboxamide-1-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Pyridinecarboxylic acid, 1-oxide | HCID 26130 | — |
| 反応物 | 4-Chloro-3-(trifluoromethyl)aniline | HCID 67574 | — |
| 反応物 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-[4-chloro-3-(trifluoromethyl)phenyl]-4-pyridinecarboxamide-1-oxide | HCID 13604808 | 56.8% |
反応手順
A suspension of isonicotinic acid 1-oxide (4.16 g, 29.9 mmol) and 1,1'-Carbonyldiimidazole (5.33 g, 32.9 mmol) in dry dimethylformamide (50 ml) was stirred for 40 minutes under an air-lock and treated with 4-chloro-3-trifluoromethylbenzenamine (6.43 g, 32.9 mmol). The reaction mixture was heated at 100° for 5.3 hours and cooled to room temperature. The solution was evaporated in vacuo and the residue triturated with ethanol (2×20 ml) to give the title compound (5.379 g), m.p. 263°-265°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04728658 |
| 出典データセット | uspto-grants-1988_03 |
| ORD ID | ord-54cd37725b2e4478be3ec63150bef675 |
| 出典メモ | uspto-grants-1988_03 |