Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,1'-Carbonyldiimidazole → Ethyl 2-amino-2-(4-trifluormethyl-3-pyridinecarbonyloxyimino)-acetate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 반응물 | 3-Pyridinecarboxylic acid, 4-(trifluoromethyl)- | HCID 2777549 | — |
| 반응물 | Ethoxycarbonylformamide oxime | HCID 136108985 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | Ethyl 2-amino-2-(4-trifluormethyl-3-pyridinecarbonyloxyimino)-acetate | HCID 73994277 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06239160B1 |
| 출처 데이터셋 | uspto-grants-2001_05 |
| ORD ID | ord-0796637d1f214032bedd7a3eb5fa0941 |
| 출처 메모 | uspto-grants-2001_05 |