HRID1196982

反应详情

EQUATION

反应方程式

HRID 1196982 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

In this example, 348.9 g of sodium salt of methyl p-hydroxybenzoate, 402.4 g of phthalide and 200 g of sodium chloride are mixed with one another and stirred at 150° C. for 6 hours. After completion of the reaction, the mixture is cooled until the temperature is brought back to room temperature, 4 l of aqueous 10% acetic acid solution is added thereto and the mixture is allowed to stand at room temperature overnight. After stirring the mixture at room temperature for 3 hours, deposited crystals are separated by filtration, and 6 l of water is added thereto. After stirring the mixture at room temperature for 30 minutes, the deposited crystals are separated by filtration. After the addition of 3 l of toluene to the crystals, the mixture is stirred at room temperature for one hour. The crystals are separated by filtration and dried over heating under reduced pressure to yield 393.9 g of 2-(4-methoxycarbonylphenoxy) methyl benzoic acid.

WORKUP

后处理

  1. customAfter completion of the reaction
  2. temperaturethe mixture is cooled until the temperature
  3. customis brought back to room temperature
  4. waitto stand at room temperature overnight
  5. stirringAfter stirring the mixture at room temperature for 3 hours
  6. customare separated by filtration, and 6 l of water
  7. additionis added
  8. stirringAfter stirring the mixture at room temperature for 30 minutes
  9. customthe deposited crystals are separated by filtration
  10. additionAfter the addition of 3 l of toluene to the crystals
  11. stirringthe mixture is stirred at room temperature for one hour
  12. customThe crystals are separated by filtration
  13. customdried
  14. temperatureover heating under reduced pressure