反应 #1856231
ord-f10de9f0097844afabdf27ad78f46ce1
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度to reflux under nitrogen for 1 hour
- 2温度The reaction mixture was cooled to room temperature
- 3过滤filtered
- 4洗涤the residual solid was washed with 500 ml of ether
- 5浓缩The combined filtrate was concentrated in vacuo
- 6workup.DISSOLUTIONthe residue was redissolved in ether
- 7洗涤the ether solution was washed successively with water and brine
- 8其他dried
- 9浓缩The solvent was concentrated
- 10workup.DISTILLATIONthe residual liquid was distilled
实验过程
A mixture of 116 g (1 mol) of 2-ethylbutyric acid, 135 g (1.05 mol) of dimethyl sulfate, and 155 g (1.12 mol) of potassium carbonate in 500 ml of acetone was stirred at room temperature under nitrogen overnight, and then was allowed to reflux under nitrogen for 1 hour. The reaction mixture was cooled to room temperature, filtered, and the residual solid was washed with 500 ml of ether. The combined filtrate was concentrated in vacuo, the residue was redissolved in ether, the ether solution was washed successively with water and brine and then dried. The solvent was concentrated and the residual liquid was distilled to afford 70 g (53.8 %) of methyl 2-ethylbutyrate, b.p. 135°-137° C.