반응 #5720

ord-f9b363bf630049efa482b18098a1d4e7

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도at reflux
  2. 2
    workup.DISTILLATIONAfter distillation of the methanol the residue
  3. 3
    workup.ADDITIONwas poured on to ice-water
  4. 4
    추출It was then extracted with n-hexane and water
  5. 5
    기타dried
  6. 6
    기타After evaporation of the solvent
  7. 7
    workup.DISTILLATIONdistillation there

실험 절차

465 g of methyl acetoacetate and then 458 g of ethyl bromide were added under nitrogen to 720 g of 30% sodium methylate solution in 1200 ml of methanol. The reaction mixture was subsequently boiled at reflux. After distillation of the methanol the residue was poured on to ice-water. It was then extracted with n-hexane and water. The organic phases were combined and dried. After evaporation of the solvent and distillation there were obtained 328 g (56.9%) of methyl 2-acetylbutyrate, b.p. 77°-79°/15 Torr.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05245056uspto-grants-1993_09