HRID430565

反应详情

EQUATION

反应方程式

HRID 430565 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of ethyl 4-hydroxy-7-(trifluoromethyl)-3-quinolinecarboxylate (43.4 g, 0.521 mol) and 10% sodium hydroxide (150 mL) was heated to reflux. Most of the ester did not dissolve so methanol (150 mL) was added over the course of an hour to facilitate dissolution. After refluxing for 2 hours a solution was obtained. The solution was refluxed for an additional 2 hours and then allowed to cool to ambient temperature overnight. The methanol was removed under reduced pressure and the resulting aqueous solution was acidified with concentrated hydrochloric acid. The resulting precipitate was isolated by filtration, washed with water and then dried in a vacuum oven at 120° C. for 24 hours to provide 38.5 g of 4-hydroxy-7-(trifluoromethyl)-3-quinolinecarboxylic acid as a white solid.

WORKUP

后处理

  1. temperaturewas heated to reflux
  2. additionwas added over the course of an hour
  3. dissolutiondissolution
  4. temperatureAfter refluxing for 2 hours a solution
  5. customwas obtained
  6. temperatureThe solution was refluxed for an additional 2 hours
  7. customThe methanol was removed under reduced pressure
  8. customThe resulting precipitate was isolated by filtration
  9. washwashed with water
  10. customdried in a vacuum oven at 120° C. for 24 hours