HRID1250497

反应详情

EQUATION

反应方程式

HRID 1250497 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.0 g (0.0032 mol) of 4-methoxy-6-{3-(trifluoromethyl)phenoxy}-2-pyridine carboxamide was dissolved in benzene and mixed with 0.93 g (0.0032×2.0 mol) of chloral, followed by treating the obtained solution under reflux for about 5 hours. The reaction solution was concentrated and then distributed in ethyl acetate-saturated sodium bicarbonate water, followed by washing with saturated brine. The organic phase of the obtained solution was dried with anhydrous sodium sulfate, concentrated and purified by silica gel column chromatography (eluting solution: ethyl acetate/hexane), thereby obtaining an aimed product.

WORKUP

后处理

  1. additionby treating the obtained solution
  2. temperatureunder reflux for about 5 hours
  3. concentrationThe reaction solution was concentrated
  4. washby washing with saturated brine
  5. dry with materialThe organic phase of the obtained solution was dried with anhydrous sodium sulfate
  6. concentrationconcentrated
  7. custompurified by silica gel column chromatography (eluting solution: ethyl acetate/hexane)