Sodium Carbonate → 4-(6-Chloropyrimidin-4-yl)-1,4-oxazepane
反応式
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]=1参加物
5
実験手順
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)
後処理
- 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
出典と根拠
- ORDレコード
- ord-ec22e14b7acc48e89d69003ca983711d
- 出典データセット
- uspto-grants-2013_11
- 特許番号
- US08580778B2
反応ノート
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