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Sodium Hydroxide → 1-(o-Fluorophenyl)-5-(p-nitrophenyl)-1H-1,2,4-triazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Hydrazine, (2-fluorophenyl)-, hydrochloride (1:1) | HCID 2723910 | — |
| 反応物 | N-(dimethylaminomethylene)-p-nitrobenzamide | HCID 12550338 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 1-(o-Fluorophenyl)-5-(p-nitrophenyl)-1H-1,2,4-triazole | HCID 23469722 | — |
反応手順
A 25.0 g. portion of o-fluorophenylhydrazine hydrochloride is dissolved in 150 ml. of p-dioxane with warming and 31.0 ml. of 5 N sodium hydroxide is added. After solution is complete, 80 ml. of glacial acetic acid and 210 ml. of water are added followed by 28.1 g. of N-(dimethylaminomethylene)-p-nitrobenzamide in 100 ml. of warm p-dioxane. This reaction mixture is heated at 90°-95° C. for 1.5 hours, then cooled and poured into 1500 ml. of water. The solid is collected by filtration, washed with water, dried and crystallized from 200 ml. of ethanol, giving 13.9 g. of the desired product as a tan solid, mp. 143°-145° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04259504 |
| 出典データセット | uspto-grants-1981_03 |
| ORD ID | ord-769e086f96e04461b8f8105605192835 |
| 出典メモ | uspto-grants-1981_03 |