Pyrazole → 1-(ethoxymethyl)-1H-pyrazole
反応式
[NH:1]1[CH:5]=[CH:4][CH:3]=[N:2]1.C(=O)([O-])[O-].[K+].[K+].[CH2:12]([O:14][CH2:15]Cl)[CH3:13]>CC(C)=O>[CH2:12]([O:14][CH2:15][N:1]1[CH:5]=[CH:4][CH:3]=[N:2]1)[CH3:13]参加物
5
反応条件
- 温度
- 0 °C
実験手順
To a mixture of pyrazole (10 g, 0.150 mol) and potassium carbonate (22.3 g, 0.162 mol) in acetone (200.0 mL), cooled to 0° C. under nitrogen, was added chloromethyl ethyl ether (15.0 mL, 0.162 mol) via syringe over a period of 20 minutes. The reaction was stirred for 30 minutes at 0° C. and then for 2 hours at room temperature. The mixture was filtered, washing the solid with acetone (200.0 mL). The filtrate was carefully concentrated in vacuo (at 400 mbar). The crude material was purified by flash column chromatography eluting with pentane:diethylether (1:1, by volume) to afford the title compound as a colourless oil, 9.3 g, 50% yield.
後処理
- waitfor 2 hours at room temperature
- filtrationThe mixture was filtered
- washwashing the solid with acetone (200.0 mL)
- concentrationThe filtrate was carefully concentrated in vacuo (at 400 mbar)
- customThe crude material was purified by flash column chromatography
- washeluting with pentane:diethylether (1:1, by volume)
出典と根拠
- ORDレコード
- ord-e0460eb9b009438f88eda994a318d272
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08541588B2
反応ノート
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