HRID1532790

反应详情

EQUATION

反应方程式

HRID 1532790 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

First, 20.0 g of methylmalonic acid diethyl ester was dissolved in a mixed solution of 30 g of water and 30 g of ethanol. To this solution was added dropwise 9.6 g of 48% aqueous NaOH solution, and the mixture was vigorously stirred at room temperature for 7 hours. After completion of the reaction, the reaction solution was adjusted to pH 3 by the addition of 35% hydrochloric acid and concentrated under reduced pressure. To the residue was added 80 g of water, and the mixture was extracted twice with 40 g of ethyl acetate. The organic layers were combined and concentrated under reduced pressure. To the residue was added 100 g of n-hexane, and the precipitated crystals were collected by filtration. The filtrate was concentrated under reduced pressure to give 16.1 g of methylmalonic acid monoethyl ester.

WORKUP

后处理

  1. customAfter completion of the reaction
  2. concentrationconcentrated under reduced pressure
  3. additionTo the residue was added 80 g of water
  4. extractionthe mixture was extracted twice with 40 g of ethyl acetate
  5. concentrationconcentrated under reduced pressure
  6. additionTo the residue was added 100 g of n-hexane
  7. filtrationthe precipitated crystals were collected by filtration
  8. concentrationThe filtrate was concentrated under reduced pressure