Sodium Carbonate → 4-(6-Chloropyrimidin-4-yl)-1,4-oxazepane
반응식
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[CH:4][N:3]=1.Cl.[O:10]1[CH2:16][CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1.C(=O)([O-])[O-].[Na+].[Na+]>O>[Cl:8][C:6]1[N:5]=[CH:4][N:3]=[C:2]([N:13]2[CH2:14][CH2:15][CH2:16][O:10][CH2:11][CH2:12]2)[CH:7]=1참가 물질
5
실험 절차
A mixture of 3.0 g (20.1 mmol) of 4,6-dichloropyrimidine, 2.8 g (20.1 mmol) of 1,4-oxazepane hydrochloride and 6.4 g (60.4 mmol) of sodium carbonate in 45 ml of water is stirred under reflux for 16 h. After cooling to RT, the reaction mixture is extracted with ethyl acetate. The organic phase is washed with saturated sodium chloride solution, dried over sodium sulphate and filtered. Under reduced pressure, the filtrate is concentrated to dryness. The product is obtained as an oil. Yield: 3.9 g (86% of theory)
후처리
- temperatureunder reflux for 16 h
- extractionthe reaction mixture is extracted with ethyl acetate
- washThe organic phase is washed with saturated sodium chloride solution
- dry with materialdried over sodium sulphate
- filtrationfiltered
- concentrationUnder reduced pressure, the filtrate is concentrated to dryness
- customThe product is obtained as an oil
출처 및 근거
- ORD 기록
- ord-ec22e14b7acc48e89d69003ca983711d
- 출처 데이터셋
- uspto-grants-2013_11
- 특허 번호
- US08580778B2
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