Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → Ethyl 1-(6-chloropyridin-2-yl)-5-(trifluoromethyl)-1h-pyrazole-4-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2-Chloro-6-hydrazinopyridine | HCID 320004 | — |
| 반응물 | Ethyl 2-(ethoxymethylene)-4,4,4-trifluoro-3-oxobutanoate | HCID 4685753 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | Ethyl 1-(6-chloropyridin-2-yl)-5-(trifluoromethyl)-1h-pyrazole-4-carboxylate | HCID 73012968 | — |
반응 단계
To a solution 2-chloro-6-hydrazinopyridine (1.00 g, 6.97 mmol) and triethylamine (0.971 mL, 6.97 mmol) in acetonitrile (35 mL) was added ethyl 2-(ethoxymethylene)-4,4,4-trifluoro-3-oxobutyrate (1.36 mL, 6.97 mmol). After 20 min, the reaction mixture was placed in a 60° C. oil bath. After 30 min, the reaction mixture was allowed to cool to ambient temperature, then was concentrated in vacuo. Purification by flash chromatography on silica gel (0 to 30% EtOAc in hexanes, then 30 to 100% EtOAc in hexanes) gave the title compound: LCMS m/z 319.9 [M+H]+; 1H NMR (500 MHz, CDCl3) δ 8.10 (s, 1 H),7.88 (t, J=7.5 Hz, 1 H),7.58 (d, J=8.0 Hz, 1 H),7.47 (d, J=8.0 Hz, 1 H),4.38 (q, J=7.0 Hz, 2 H),1.38 (t, J=7.0 Hz, 3 H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08895583B2 |
| 출처 데이터셋 | uspto-grants-2014_11 |
| ORD ID | ord-baf8ec754cbb4514945083ead0ed1075 |
| 출처 메모 | uspto-grants-2014_11 |