反応式
[Mg].Br[CH:3](C)C.C([Mg]Br)(C)C.[CH3:11][O:12][C:13]1[C:18]([CH:19]=O)=[C:17]([O:21][CH3:22])[N:16]=[CH:15][N:14]=1.[Cl-].[NH4+].[O:25]1[CH2:29][CH2:28][CH2:27]C1>>[CH3:11][O:12][C:13]1[C:18]([CH2:19][CH:29]([OH:25])[CH:28]([CH3:3])[CH3:27])=[C:17]([O:21][CH3:22])[N:16]=[CH:15][N:14]=1参加物
実験手順
0.81 g (33 mmol) of magnesium was added to 30 ml of tetrahydrofuran, and 4.1 g (33 mmol) of 2-bromopropane was added to prepare a tetrahydrofuran solution of isopropyl magnesium bromide. 2.8 g (17 mmol) of 4,6-dimethoxypyrimidine-5-carboaldehyde was dissolved in 50 ml of tetrahydrofuran, and the solution was added to the above tetrahydrofuran solution at room temperature and reacted overnight. The reaction solution was poured into an aqueous ammonium chloride solution and extracted with ethyl acetate. The organic layer was washed with an aqueous citric acid solution, water and an aqueous sodium chloride solution in this order, dried and concentrated, and the obtained oily product was purified by column chromatography (ethyl acetate:n-hexane=1:4) to obtain 1.9 g (yield: 54%) of 1-(4,6-dimethoxy pyrimidin-5-yl)-3-methylbutan-2-ol as slightly yellow crystals.
後処理
- additionwas added
- customreacted overnight
- extractionextracted with ethyl acetate
- washThe organic layer was washed with an aqueous citric acid solution, water
- dry with materialan aqueous sodium chloride solution in this order, dried
- concentrationconcentrated
- customthe obtained oily product was purified by column chromatography (ethyl acetate:n-hexane=1:4)
出典と根拠
- ORDレコード
- ord-d022aedc6a5e46c7be25577186f30d77
- 出典データセット
- uspto-grants-2004_10
- 特許番号
- US06806230B1
関連ノート
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