HRID354633

反应详情

EQUATION

反应方程式

HRID 354633 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

6.6 g (0.06 mol) of m-aminophenol in 4.0 g (0.06 mol) of 85% potassium hydroxide and 80 ml of dimethylsulfoxide was heated under stirring. The water generated was distilled away under reduced pressure to make the potassium m-aminophenolate. To the solution which was allowed to cool to room temperature was added a solution of 11.9 g (0.06 mol) of 2,6-dichloroquinoxaline dissolved in 80 ml of dioxane. The mixture was reacted at 50°-60° C. for 5 hours. After the reaction was over, the reaction mixture was poured into ice and cold water. The formed solid was filtered off and washed with 5% aqueous solution of sodium hydroxide and then washed with water. The crude crystals thus obtained were recrystallized from ethanol, to produce 8.8 g (yield 54%) of white crystals, m.p. 119°-120° C.

WORKUP

后处理

  1. distillationThe water generated was distilled away under reduced pressure
  2. customThe mixture was reacted at 50°-60° C. for 5 hours
  3. filtrationThe formed solid was filtered off
  4. washwashed with 5% aqueous solution of sodium hydroxide
  5. washwashed with water
  6. customThe crude crystals thus obtained
  7. customwere recrystallized from ethanol