Imidazole → ethyl 2-(1H-imidazol-1-yl)acetate
反応式
[Na].[NH:2]1[CH:6]=[CH:5][N:4]=[CH:3]1.Br[CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10]>C(O)C>[N:2]1([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:6]=[CH:5][N:4]=[CH:3]1参加物
5
実験手順
118.2 g (5.1 mmol) of sodium are added slowly to 2.5 litres of ethanol. 350.0 g (5.1 mol) of imidazole and 570 ml (858.6 g, 5.1 mol) of ethyl bromoacetate are added dropwise at an internal temperature of 20-25° C. The mixture is stirred at RT for 24 h. The precipitated solid is filtered off, the ethanol is removed under reduced pressure and the mixture is filtered again. The residue is purified by column chromatography on silica gel (mobile phase ethyl acetate). Yield: 639.0 g (81% of theory)
後処理
- filtrationThe precipitated solid is filtered off
- customthe ethanol is removed under reduced pressure
- filtrationthe mixture is filtered again
- customThe residue is purified by column chromatography on silica gel (mobile phase ethyl acetate)
出典と根拠
- ORDレコード
- ord-2c36d1f0258c4a30833050141901c87b
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08067407B2
反応ノート
読み込み中…