関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Chloro-4-methylaniline | HCID 7255 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-Methyl-4-imidazolecarbonyl chloride hydrochloride | HCID 20268027 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | N-(3-chloro-4-methylphenyl)-5-methyl-4-imidazolecarboxamide | HCID 20268024 | 85% |
反応手順
To a solution of 740 g (5.22 moles) of 3-chloro-4-methylaniline and 1054.6 g (10.44 moles) of triethylamine in 10 liters of acetone at room temperature and vigorous stirring, there were added slowly 945 g (5.22 moles) of 5-methyl-4-imidazolecarbonyl chloride hydrochloride. After the addition was ended, the mixture was refluxed for 1 hour and then allowed to cool to room temperature and filtered. The liquid filtrate was evaporated until a slight precipitation appeared, it was then poured over 20 liters of cold water with stirring, filtered and the precipitate was dried to give N-(3-chloro-4-methylphenyl)-5-methyl-4-imidazolecarboxamide, a crude yellowish product. Crystallisation from isopropyl alcohol gave 1108 g (85% yield) of the desired pure product having the same characteristics as the one obtained in Example 1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04539331 |
|---|
| 出典データセット | uspto-grants-1985_09 |
|---|
| ORD ID | ord-094e7fc328a54ec49c142b95a8c3acb3 |
|---|
| 出典メモ | uspto-grants-1985_09 |
|---|