참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-Butanol | HCID 263 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | (S)-1-(4-Fluorophenyl)-ethylamine | HCID 2779063 | — |
| 반응물 | (S)-6-(5-Cyclopropyl-1H-pyrazol-3-ylamino)-5-fluoro-2-(1-(4-fluorophenyl)ethylamino)nicotinamide | HCID 67455185 | — |
| 생성물 | HCID 178458645 | HCID 178458645 | 48% |
반응 단계
2-Chloro-5-fluoro-6-(5-isopropoxy-1H-pyrazol-3-ylamino)nicotinonitrile (Method 2; 1.4 g, 5.0 mmol) and (S)-1-(4-fluorophenyl)ethanamine (1.0 g, 9.0 mmol) were added to a solution of n-BuOH (8 ml) and DIEA (0.8 g, 6.0 mmol) in a sealed tube. The reaction was heated to 135° C. for 48 hrs, cooled to 25° C., and concentrated. The resulting residue was purified by column chromatography (DCM-MeOH=80:1) to give the title compound (0.90 g, 48%). 1H NMR (400 MHz, CD3OD) δ 7.43 (d, J=10.5 Hz, 1H), 7.39-7.35 (m, 2H), 7.04-6.99 (m, 2H), 5.47 (s, 1H), 5.12-5.11 (m, 1H), 4.60-4.51 (m, 1H), 1.56 (d, J=7.0 Hz, 3H), 1.33-1.30 (m, 6H). MS: Calcd.: 398. Found: [M+H]+ 399.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08835465B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_09 |
|---|
| ORD ID | ord-7eed2fd2a9744cafbb38b9dc96fedbde |
|---|
| 출처 메모 | uspto-grants-2014_09 |
|---|
