HRID1073021

反应详情

EQUATION

反应方程式

HRID 1073021 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 7.25 mmol of 2-(4-((6-chloro-2-quinoxalinyl)oxy)phenoxy)propionyl chloride, prepared using substantially the procedure of Step A of Example 1 from the corresponding acid, in 20 ml of acetonitrile was added to solution of 1.43 g (7.25 mmol) of 4-aminobenzotrifluoride, hydrochloride and 1.83 g (18.1 mmol) of triethylamine in 10 ml of acetonitrile. The reaction mixture was warmed at reflux for a period of 4 hours and then poured over crushed ice. The resulting precipitate was collected by filtration and then recrystallized from acetonitrile to give 2.40 g (68 percent of theoretical) of the above-named product as a tan solid which melted at 176°-178° C. The structure of the product was confirmed by its IR and NMR spectrum. (Compound 5)

WORKUP

后处理

  1. temperatureThe reaction mixture was warmed
  2. temperatureat reflux for a period of 4 hours
  3. additionpoured
  4. customover crushed ice
  5. filtrationThe resulting precipitate was collected by filtration
  6. customrecrystallized from acetonitrile