반응식
Br[C:2]1[N:7]=[C:6]([N:8]2[CH2:14][CH2:13][CH2:12][N:11]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:10][CH2:9]2)[CH:5]=[CH:4][CH:3]=1.[Cl:22][C:23]1[N:28]=[CH:27][C:26]2[CH:29]=[N:30][NH:31][C:25]=2[CH:24]=1.C([O-])([O-])=O.[K+].[K+].CNCCNC>O1CCOCC1.[Cu]I>[Cl:22][C:23]1[N:28]=[CH:27][C:26]2[CH:29]=[N:30][N:31]([C:2]3[N:7]=[C:6]([N:8]4[CH2:14][CH2:13][CH2:12][N:11]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:10][CH2:9]4)[CH:5]=[CH:4][CH:3]=3)[C:25]=2[CH:24]=1참가 물질
7
반응물 4
생성물 1
시약·촉매·용매 2
반응 조건
- 온도
- 100 °C
실험 절차
To a mixture of tert-butyl 4-(6-bromopyridin-2-yl)-1,4-diazepane-1-carboxylate (2.55 g, 7.16 mmol) and 6-chloro-1H-pyrazolo[4,3-c]pyridine (1.0 g, 6.51 mmol) in 1,4-dioxane (20 mL) was added CuI (494 mg, 2.6 mmol), K2CO3 (3.6 g, 26 mmol), and N1,N2-dimethylethane-1,2-diamine (460 mg, 5.2 mmol). The mixture was heated at 100° C. for 3 hours, which was monitored by LCMS. After completion of the reaction, it was concentrated under reduced pressure. The crude was purified by silica gel chromatography using petroleum ether/EtOAc (2/1) as eluting solvents to afford tert-butyl 4-(6-(6-chloro-1H-pyrazolo[4,3-c]pyridin-1-yl)pyridin-2-yl)-1,4-diazepane-1-carboxylate as a yellow solid (1.6 g, 57%). MS (ESI) m/z: 429 [M+H]+.
후처리
- customAfter completion of the reaction, it
- concentrationwas concentrated under reduced pressure
- customThe crude was purified by silica gel chromatography
- washas eluting solvents
출처 및 근거
- ORD 기록
- ord-1943d0852c264f4d8db42f973130b916
- 출처 데이터셋
- uspto-grants-2016_09
- 특허 번호
- US09434725B2
연결된 노트
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