Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methylamine → N-[(3R,6S)-6-(2,3-Difluorophenyl)-2-(methylimino)-1-(2,2,2-trifluoroethyl)azepan-3-yl]-4-(2-oxo-2,3-dihydro-1H-imidazo[4,5-b]pyridin-1-yl)piperidine-1-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methylamine | HCID 6329 | — |
| 반응물 | N-[(3R,6S)-6-(2,3-Difluorophenyl)-2-thioxo-1-(2,2,2-trifluoroethyl)azepan-3-yl]-4-(2-oxo-2,3-dihydro-1H-imidazo[4,5-b]pyridin-1-yl)piperidine-1-carboxamide | HCID 86616758 | — |
| 촉매 | Mercuric Chloride | HCID 24085 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | N-[(3R,6S)-6-(2,3-Difluorophenyl)-2-(methylimino)-1-(2,2,2-trifluoroethyl)azepan-3-yl]-4-(2-oxo-2,3-dihydro-1H-imidazo[4,5-b]pyridin-1-yl)piperidine-1-carboxamide | HCID 11692732 | — |
반응 단계
Mercury(II) chloride (23 mg, 0.084 mmol) was added to a solution of N-[(3R,6S)-6-(2,3-difluorophenyl)-2-thioxo-1-(2,2,2-trifluoroethyl)azepan-3-yl]-4-(2-oxo-2,3-dihydro-1H-imidazo[4,5-b]pyridin-1-yl)piperidine-1-carboxamide (32 mg, 0.055 mmol) and methylamine (2.0 M in tetrahydrofuran; 274 μL, 0.547 mmol) in ethanol (1 mL). After 2 h, the mixture was filtered and concentrated. Purification by reverse phase HPLC(C-18, 95% water/acetonitrile→100% acetonitrile with 0.1% trifluoroacetic acid) gave the title compound as a bis trifluoroacetate salt (33 mg). MS 580.2415 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07732438B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-bdbb0e01efff449995836e535d094a93 |
| 출처 메모 | uspto-grants-2010_06 |