HRID1250498

反应详情

EQUATION

反应方程式

HRID 1250498 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

1.0 g (0.0022 mol) of N-(1-hydroxy-2,2,2-trichloroethyl)-4-methoxy-6-{3-(trifluoromethyl)phenoxy}-2-pyridine carboxamide was dissolved in about 10 ml of acetic acid. The obtained solution was mixed with 0.29 g (0.0022×2.0 mol) of zinc dust and stirred at about 50° C. for about 5 hours. The reaction solution was distributed in ethyl acetate-water and washed with saturated sodium bicarbonate water and saturated brine. The organic phase of the 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. washwashed with saturated sodium bicarbonate water and saturated brine
  2. dry with materialThe organic phase of the solution was dried with anhydrous sodium sulfate
  3. concentrationconcentrated
  4. custompurified by silica gel column chromatography (eluting solution: ethyl acetate/hexane)