HRID1266923

反应详情

EQUATION

反应方程式

HRID 1266923 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Then, a reaction flask was loaded with acetic acid (30 ml) and 9,10-phenanthrenequinone (2.0 g), and the temperature was raised to 100° C. with stirring to dissolve 9,10-phenanthrenequinone. To this mixture, 2-hydrazino-6-(4-trifluoromethylphenoxy)pyridine (3.0 g) was added in 15 minutes. After stirring at 95 to 105° C. for two hours, the reaction mixture was filtrated. The filtrated crystals were successively washed with hot water and hot methanol, followed by recrystallization with dioxane-water to give crystals, which were then filtrated and dried to give intended crystals (3.5 g).

WORKUP

后处理

  1. stirringAfter stirring at 95 to 105° C. for two hours
  2. filtrationthe reaction mixture was filtrated
  3. washThe filtrated crystals were successively washed with hot water and hot methanol
  4. customfollowed by recrystallization with dioxane-water
  5. customto give crystals, which
  6. filtrationwere then filtrated
  7. customdried
  8. customto give