Water → 2-(6-Azidopyrimidin-4-yloxy)ethanol
反応式
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]([O:8][CH2:9][CH2:10][OH:11])[CH:3]=1.[N-:12]=[N+:13]=[N-:14].[Na+].O>CN(C)C=O>[N:12]([C:2]1[N:7]=[CH:6][N:5]=[C:4]([O:8][CH2:9][CH2:10][OH:11])[CH:3]=1)=[N+:13]=[N-:14]参加物
5
反応条件
- 温度
- 70 °C
実験手順
To a solution of 2-(6-chloropyrimidin-4-yloxy)ethanol (5.61 g) in dimethylformamide (60 ml) is added sodium azide (4.18 g), and the mixture is stirred at 70° C. for 20 hours. After cooling, the reaction solution is treated with water, and extracted with ethyl acetate. The ethyl acetate layer is dried, and evaporated to remove the solvent. The residue is purified by silica gel column chromatography (solvent; hexane/ethyl acetate=1:1) to give 2-(6-azidopyrimidin-4-yloxy)ethanol (1.68 g).
後処理
- temperatureAfter cooling
- extractionextracted with ethyl acetate
- dry with materialThe ethyl acetate layer is dried
- customevaporated
- customto remove the solvent
- customThe residue is purified by silica gel column chromatography (solvent; hexane/ethyl acetate=1:1)
出典と根拠
- ORDレコード
- ord-fca1a49f76c14ce8bae2a93158f456ab
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05728706
反応ノート
読み込み中…