HRID434526

反应详情

EQUATION

反应方程式

HRID 434526 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 22 g of the product of Step A, 220 ml of ethanol and 110 ml of sodium hydroxide was stirred at room temperature for 36 hours and the ethanol was then evaporated at less than 40° C. under reduced pressure. The solution was diluted with 200 ml of water and ice and the pH was adjusted to 1 by addition of concentrated hydrochloric acid. The mixture was vacuum filtered and the product was washed with water and then was dissolved in ether. The solution was filtered and the filtrate was dried and evaporated to dryness under reduced pressure to obtain 18 g of 2-dichloromethyl-4-hydroxy-8-trifluoromethyl-3-quinoline-carboxylic acid which was used as is for the next step.

WORKUP

后处理

  1. customthe ethanol was then evaporated at less than 40° C. under reduced pressure
  2. additionThe solution was diluted with 200 ml of water and ice
  3. additionthe pH was adjusted to 1 by addition of concentrated hydrochloric acid
  4. filtrationfiltered
  5. washthe product was washed with water
  6. dissolutionwas dissolved in ether
  7. filtrationThe solution was filtered
  8. customthe filtrate was dried
  9. customevaporated to dryness under reduced pressure