HRID742997

反应详情

EQUATION

反应方程式

HRID 742997 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Methyl 2-hydroxy-5-[2-[4-[(2-pyridinylamino)sulfonyl]phenyl]ethenyl]benzoate (12 g, 29 mmol) was dissolved in 1M KOH (120 ml) and the solution was refluxed for 7 h. The cooled solution was acidified with an excess of 1M hydrochloric acid. The precipitate was filtered off and washed with water (3×200 ml). The product was redissolved in a small portion of 1M NaOH. Water and dioxane (500+500 ml) was added and the solution was heated to 100° C. The solution was acidified with an excess of 1M HCl, and the product precipitated upon cooling. Yield 9 g (75%).

WORKUP

后处理

  1. temperaturethe solution was refluxed for 7 h
  2. filtrationThe precipitate was filtered off
  3. washwashed with water (3×200 ml)
  4. dissolutionThe product was redissolved in a small portion of 1M NaOH
  5. additionWater and dioxane (500+500 ml) was added
  6. customthe product precipitated
  7. temperatureupon cooling