HRID5624

反应详情

EQUATION

反应方程式

HRID 5624 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. temperatureat reflux
  2. distillationAfter distillation of the methanol the residue
  3. additionwas poured on to ice-water
  4. extractionIt was then extracted with n-hexane and water
  5. customdried
  6. customAfter evaporation of the solvent
  7. distillationdistillation there