Sodium hydride → 1-(Pyrazin-2-yl)-1H-imidazole-4-carbaldehyde
반응식
[H-].[Na+].[NH:3]1[CH:7]=[C:6]([CH:8]=[O:9])[N:5]=[CH:4]1.Cl[C:11]1[CH:16]=[N:15][CH:14]=[CH:13][N:12]=1>CN(C=O)C>[N:12]1[CH:13]=[CH:14][N:15]=[CH:16][C:11]=1[N:3]1[CH:7]=[C:6]([CH:8]=[O:9])[N:5]=[CH:4]1참가 물질
5
반응 조건
- 온도
- 0 °C
실험 절차
Sodium hydride (60% in oil, 720 mg, 18.0 mmol) was added to a 0° C. solution of 1H-imidazole-4-carboxaldehyde (2.20 g, 18.0 mmol) in DMF (8 mL). After stirring for 20 min at 0° C., the mixture was allowed to warm to RT and a solution of 2-chloropyrazine (2.06 g, 17.9 mmol) in DMF (4 mL) was added. The resulting mixture was heated to 100° C. for 18 h. The solvent was evaporated, the residue was dissolved in ethyl acetate, washed with water and brine, dried (MgSO4), and concentrated to provide 3.10 g (86%) of the title compound. MS 175 (M+H)+
후처리
- temperatureto warm to RT
- temperatureThe resulting mixture was heated to 100° C. for 18 h
- customThe solvent was evaporated
- dissolutionthe residue was dissolved in ethyl acetate
- washwashed with water and brine
- dry with materialdried (MgSO4)
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-0326d4b48151442e9091b15321845211
- 출처 데이터셋
- uspto-grants-2004_03
- 특허 번호
- US06713455B2
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