Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
3-Pyridinecarboxylic acid, 4-(trifluoromethyl)- → Tert-butyl 3-amino-3-(4-trifluoromethyl-3-pyridinecarbonyloxyimino)propionate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 3-Pyridinecarboxylic acid, 4-(trifluoromethyl)- | HCID 2777549 | — |
| 반응물 | Bis-(1H-imidazol-2-YL)-methanone | HCID 5250894 | — |
| 반응물 | tert-butyl 2-(N'-hydroxycarbamimidoyl)acetate | HCID 76589802 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Tert-butyl 3-amino-3-(4-trifluoromethyl-3-pyridinecarbonyloxyimino)propionate | HCID 53931299 | 51.6% |
반응 단계
30 g of 4-trifluoromethyl-3-pyridinecarboxylic acid is initially charged in 150 ml of dry THF and, a little at a time, admixed with 25.3 g of carbonyl-diimidazole. The mixture is stirred at room temperature for 30 min. 27.2 g of tert-butoxycarbonylacetamide oxime dissolved in 150 ml of THF are then added dropwise. The mixture is stirred overnight, the solvent is evaporated and the residue is taken up in ethyl acetate, washed three times with 1 M sulfuric acid and once with saturated sodium bicarbonate solution. Concentration of the ethyl acetate phase gives 28 g of the product as a pale yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06239160B1 |
| 출처 데이터셋 | uspto-grants-2001_05 |
| ORD ID | ord-fdaa577ba9fd42aa8988ed42e6d7917c |
| 출처 메모 | uspto-grants-2001_05 |