반응식
C([Li])CCC.CCCCCC.Br[C:13]1[C:14]([O:21][CH3:22])=[N:15][C:16]([O:19][CH3:20])=[N:17][CH:18]=1.[Cl:23][C:24]1[CH:25]=[C:26]2[C:30](=[CH:31][CH:32]=1)[NH:29][C:28](=[O:33])[C:27]2=[O:34].[Cl-].[NH4+]>C1COCC1>[Cl:23][C:24]1[CH:25]=[C:26]2[C:30](=[CH:31][CH:32]=1)[NH:29][C:28](=[O:33])[C:27]2([C:13]1[C:14]([O:21][CH3:22])=[N:15][C:16]([O:19][CH3:20])=[N:17][CH:18]=1)[OH:34]참가 물질
반응 조건
- 온도
- -78 °C
실험 절차
A 1.6 M solution of n-butyllithium in hexane (10 ml, 16 mmol) was added dropwise to a solution of 5-bromo-2,4-dimethoxypyrimidine (3.29 g, 15 mmol) in THF (50 ml) at −78° C. After stirring at −78° C. for 0.5 h, a suspension of 5-chloroisatin (1.27 g, 7.0 mmol) in THF (50 ml) was added dropwise. The reaction mixture was allowed to warm to room temperature and then saturated ammonium chloride solution was added. The mixture was extracted three times with ethyl acetate, and the combined organic layers were washed with saturated brine. The organic phase was dried over magnesium sulfate, filtered and concentrated under reduced pressure. Purification by chromatography (silica gel, 50% ethyl acetate in dichloromethane) resulted in 0.97 g of the intermediate.
후처리
- additionwas added dropwise
- temperatureto warm to room temperature
- extractionThe mixture was extracted three times with ethyl acetate
- washthe combined organic layers were washed with saturated brine
- dry with materialThe organic phase was dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customPurification by chromatography (silica gel, 50% ethyl acetate in dichloromethane)
출처 및 근거
- ORD 기록
- ord-7adaf7ffb7214d29a178fe10515f228e
- 출처 데이터셋
- uspto-grants-2011_03
- 특허 번호
- US07902379B2
연결된 노트
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