化工社化工社 化学情報印刷レポート · 研究参考用
1,1'-Carbonyldiimidazole → Ethyl 2-amino-2-(4-trifluormethyl-3-pyridinecarbonyloxyimino)-acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 反応物 | 3-Pyridinecarboxylic acid, 4-(trifluoromethyl)- | HCID 2777549 | — |
| 反応物 | Ethoxycarbonylformamide oxime | HCID 136108985 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Ethyl 2-amino-2-(4-trifluormethyl-3-pyridinecarbonyloxyimino)-acetate | HCID 73994277 | — |
反応手順
17.3 g of carbonyidiimidazole are initially charged in 200 ml of 1,4-dioxane and, a little at a time, admixed with 20 g of 4-trifluoromethyl-3-pyridinecarboxylic acid. The mixture is stirred at room temperature for 1 h and subsequently heated to 45° C. for 2 h. After cooling to 30° C., 14.5 g of ethoxycarbonylformamide oxime are added and the mixture is stirred at 45° C. for 3 h. The precipitated solid is filtered off with suction and the filtrate is concentrated to 50 ml and, together with the solid, added to 250 ml of ice-water. The solid is filtered off with suction and dried at 50° C. under reduced pressure. This gives 28.7 g of the product as a white solid of mp. 172-174° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06239160B1 |
| 出典データセット | uspto-grants-2001_05 |
| ORD ID | ord-0796637d1f214032bedd7a3eb5fa0941 |
| 出典メモ | uspto-grants-2001_05 |