HRID2226741

反应详情

EQUATION

反应方程式

HRID 2226741 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The above ester (0.8 g, 1.8 mmol) was dissolved in ethanol (15 ml) and a 4 N sodium hydroxide solution (2 ml) was added. The mixture was stirred vigorously at room temperature for 4 h. The solvent was evaporated in vacuo to give an oily residue. Dichloromethane (100 ml) was added and the mixture was cooled on an ice-bath. A concentrated hydrochloric acid solution (1 ml) was added. The mixture was stirred vigorously for a few minutes and the phases were separated. The organic phase was dried over sodium sulphate and the solvent was evaporated in vacuo. The residue was re-evaporated with dichloromethane, dissolved in dichloromethane and left overnight at 4° C. The solid formed was isolated by filtration to give 0.6 g of the title compound as a solid.

WORKUP

后处理

  1. customThe solvent was evaporated in vacuo
  2. customto give an oily residue
  3. temperaturethe mixture was cooled on an ice-bath
  4. stirringThe mixture was stirred vigorously for a few minutes
  5. customthe phases were separated
  6. dry with materialThe organic phase was dried over sodium sulphate
  7. customthe solvent was evaporated in vacuo
  8. customThe residue was re-evaporated with dichloromethane
  9. dissolutiondissolved in dichloromethane
  10. waitleft overnight at 4° C
  11. customThe solid formed
  12. customwas isolated by filtration