反应 #1856231

ord-f10de9f0097844afabdf27ad78f46ce1

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度to reflux under nitrogen for 1 hour
  2. 2
    温度The reaction mixture was cooled to room temperature
  3. 3
    过滤filtered
  4. 4
    洗涤the residual solid was washed with 500 ml of ether
  5. 5
    浓缩The combined filtrate was concentrated in vacuo
  6. 6
    workup.DISSOLUTIONthe residue was redissolved in ether
  7. 7
    洗涤the ether solution was washed successively with water and brine
  8. 8
    其他dried
  9. 9
    浓缩The solvent was concentrated
  10. 10
    workup.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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05380729uspto-grants-1995_01