HRID1655543

反应详情

EQUATION

反应方程式

HRID 1655543 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4.35 mmol of 2-(4-((6-chloro-2-quinoxalinyl)oxy)phenoxy)propanoyl chloride (previously prepared from 1.5 g of the corresponding acid) in 15 ml of acetonitrile was added to a mixture prepared from 1.20 g (4.35 mmol) of 4-(1,1-difluoro-2,2,2-trichloroethoxy)aniline, 0.66 g (6.5 mmol) of triethylamine and 10 ml of acetonitrile. The mixture was warmed at reflux for a period of 2.5 hours and then poured over ice and aqueous NaOH added. The resulting precipitate was filtered and dried and then recrystallized from methylcyclohexane. This left 2.2 g (84 percent of theoretical) of the above-named product as a brown solid, m.p. 139°-141° C. (Compound 36)

WORKUP

后处理

  1. additionwas added to a mixture
  2. temperatureThe mixture was warmed
  3. temperatureat reflux for a period of 2.5 hours
  4. additionadded
  5. filtrationThe resulting precipitate was filtered
  6. customdried
  7. customrecrystallized from methylcyclohexane