HRID1464175

反应详情

EQUATION

反应方程式

HRID 1464175 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 2-hydroxy-5-[2-[4-[(2-pyridinylamino)sulfonyl]phenyl]ethenyl]benzoic acid (3 g, 7.5 mmol) in tetrahydrofuran (100 ml) and acetic acid (100 ml) was hydrogenated over palladium on charcoal (10%, 0.3 g) and hydrogen at atmospheric pressure and room temperature for 27 h. The catalyst was filtered off and the solvent was evaporated. The residue was dissolved in a solution of sodium hydroxide (0.3 g) in acetone (30 ml) and water (30 ml). The solution was acidified with hydrochloric acid at ca 50° C. After cooling, the product crystallized yielding 1.6 g (52%).

WORKUP

后处理

  1. filtrationThe catalyst was filtered off
  2. customthe solvent was evaporated
  3. dissolutionThe residue was dissolved in a solution of sodium hydroxide (0.3 g) in acetone (30 ml) and water (30 ml)
  4. customwas acidified with hydrochloric acid at ca 50° C
  5. temperatureAfter cooling
  6. customthe product crystallized
  7. customyielding 1.6 g (52%)