تفاعل #5720

ord-f9b363bf630049efa482b18098a1d4e7

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةat reflux
  2. 2
    workup.DISTILLATIONAfter distillation of the methanol the residue
  3. 3
    workup.ADDITIONwas poured on to ice-water
  4. 4
    استخلاصIt was then extracted with n-hexane and water
  5. 5
    أخرىdried
  6. 6
    أخرىAfter evaporation of the solvent
  7. 7
    workup.DISTILLATIONdistillation there

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05245056uspto-grants-1993_09