Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diisopropylethylamine → (S)-6-(5-cyclopropyl-1H-pyrazol-3-ylamino)-5-fluoro-2-(1-(4-fluorophenyl)ethylamino)-4-iodonicotinonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | (S)-1-(4-Fluorophenyl)-ethylamine | HCID 2779063 | — |
| 반응물 | 2-chloro-6-(5-cyclopropyl-1H-pyrazol-3-ylamino)-5-fluoro-4-iodonicotinonitrile | HCID 86620615 | — |
| 용매 | 1-Butanol | HCID 263 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | (S)-6-(5-cyclopropyl-1H-pyrazol-3-ylamino)-5-fluoro-2-(1-(4-fluorophenyl)ethylamino)-4-iodonicotinonitrile | HCID 67456774 | 20% |
반응 단계
A solution of 2-chloro-6-(5-cyclopropyl-1H-pyrazol-3-ylamino)-5-fluoro-4-iodonicotinonitrile (Method 39, 0.28 g, 0.69 mmol), (5)-1-(4-fluorophenyl)ethanamine (0.19 g, 1.3 mmol), and DIEA (0.11 g, 0.90 mmol) in n-BuOH (1 ml) was heated to 140° C. for 18 hours. The reaction was diluted with water (10 ml), extracted with DCM (2×20 ml) and the combined organic fractions were dried over Na2SO4, filtered, and then concentrated. The resulting oil was purified by column chromatography (DCM-MeOH=100:1) to give the title compound (0.07 g, 20%). MS: Calcd.: 506. Found: [M+H]+ 507.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08835465B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-039937d44dde4b9c8b4dac5bbb19579d |
| 출처 메모 | uspto-grants-2014_09 |