反応 #74607

反応方程式

pyrazole

potassium carbonate

chloromethyl ethyl ether

→

title compound

収率 50.0%

1-(Ethoxymethyl)-1H-pyrazole

収率 50.0%

溶媒

acetone

反応条件

後処理

1. 1
   workup.WAITfor 2 hours at room temperature
2. 2
   ろ過The mixture was filtered
3. 3
   洗浄washing the solid with acetone (200.0 mL)
4. 4
   濃縮The filtrate was carefully concentrated in vacuo (at 400 mbar)
5. 5
   その他The crude material was purified by flash column chromatography
6. 6
   洗浄eluting with pentane:diethylether (1:1, by volume)

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.

出典