HRID1653902

反应详情

EQUATION

反应方程式

HRID 1653902 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ethyl 2-hydroxy-5-[[4-[(3-methyl-2-pyridinylamino)sulfonyl]phenyl]ethynyl]benzoate (15.5 g, 35 mmol) was refluxed in potassium hydroxide (10 g, 0.15 mol) in water (100 ml) for 1 h. After cooling to ca 70° C., ethyl acetate (50 ml) was added and hydrochloric acid was added to reach pH 7-8. Cooling during stirring and then filtration gave a solid that was dissolved in acetone (100 ml) and water (100 ml). The solution was acidified at ca 50° C. and cooled, filtered and washed with water. Yield 8.0 g (56%).

WORKUP

后处理

  1. temperatureAfter cooling to ca 70° C.
  2. temperatureCooling
  3. filtrationfiltration
  4. customgave a solid
  5. customwas acidified at ca 50° C.
  6. temperaturecooled
  7. filtrationfiltered
  8. washwashed with water