HRID1464175
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationThe catalyst was filtered off
- customthe solvent was evaporated
- dissolutionThe residue was dissolved in a solution of sodium hydroxide (0.3 g) in acetone (30 ml) and water (30 ml)
- customwas acidified with hydrochloric acid at ca 50° C
- temperatureAfter cooling
- customthe product crystallized
- customyielding 1.6 g (52%)