HRID1468309

反应详情

EQUATION

反应方程式

HRID 1468309 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Z-Glu-OBn (371 mg, 1 mmol) was dissolved in methylene chloride (1 ml), and CDI (180 mg, 1.1 mmol) was added to the solution. The mixture was stirred at room temperature for 30 minutes. 2-Amino-4-chlorophenol-6-sulfonic acid (223 mg, 1 mmol) and THF (1 ml) were added to the mixture. The mixture was then stirred overnight at room temperature. After the solvent was removed by distillation, the mixture was purified in accordance with the purification step A. The resulting intermediate was dissolved in a methanol-water solvent mixture. A catalytic amount of Pd/C was added to the solution. The mixture was stirred overnight at room temperature in a hydrogen atmosphere. After the catalyst was filtered off, the solvent was removed by distillation. The mixture was purified according to the purification step A to give the title compound.

WORKUP

后处理

  1. stirringThe mixture was then stirred overnight at room temperature
  2. customAfter the solvent was removed by distillation
  3. customthe mixture was purified in accordance with the purification step A
  4. dissolutionThe resulting intermediate was dissolved in a methanol-water solvent mixture
  5. additionA catalytic amount of Pd/C was added to the solution
  6. stirringThe mixture was stirred overnight at room temperature in a hydrogen atmosphere
  7. filtrationAfter the catalyst was filtered off
  8. customthe solvent was removed by distillation
  9. customThe mixture was purified
  10. customaccording to the purification step A