Ethylene Glycol → 2-[(6-Chloropyrimidin-4-yl)oxy]ethan-1-ol
反応式
[Cl:1][C:2]1[CH:7]=[C:6](Cl)[N:5]=[CH:4][N:3]=1.[CH2:9]([OH:12])[CH2:10][OH:11].[H-].[Na+]>O1CCCC1>[Cl:1][C:2]1[N:3]=[CH:4][N:5]=[C:6]([O:11][CH2:10][CH2:9][OH:12])[CH:7]=1参加物
5
実験手順
To a mixture of 4,6-dichloropyrimidine (5.0 g), ethylene glycol (100 ml) and tetrahydrofuran (100 ml)is added sodium hydride (60% dispersion-type, 1.34 g) under ice-cooling. The mixture is stirred at the same temperature for two hours, and evaporated to remove the solvent. The residue is extracted with ethyl acetate, and the ethyl acetate extract is dried, and concentrated under reduced pressure. The residue is purified by silica gel column chromatography (solvent; chloroform/ethyl acetate=5:1~2:1) to give 2-(6-chloropyrimidin-4-yloxy)ethanol (5.67 g) as an oily product.
後処理
- temperaturecooling
- customevaporated
- customto remove the solvent
- extractionThe residue is extracted with ethyl acetate
- extractionthe ethyl acetate extract
- customis dried
- concentrationconcentrated under reduced pressure
- customThe residue is purified by silica gel column chromatography (solvent; chloroform/ethyl acetate=5:1~2:1)
出典と根拠
- ORDレコード
- ord-f570953042144533ac7122491f64e455
- 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…