HRID1389733

反应详情

EQUATION

反应方程式

HRID 1389733 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.056 mole (8.56 g) 2-methyl-5-methoxy paraphenylenediamine is introduced into 850 cc isopropyl anhydrous ether to which there have been added 0.085 mole (19.7 g) silver oxide and 55 g anhydrous sodium sulfate. The mixture is agitated for two hours, maintaining the temperature thereof between 30° and 40°. After cooling, the sodium sulfate and silver are separated from the reaction mixture by filtration, and the resulting filtrate is evaporated to dryness under vacuum. The dry residue, after recrystallization from a mixture of benzene-hexane, furnishes 5.8 g 2-methoxy-5-methyl benzoquinone diimine, which has a melting point of 96°.

WORKUP

后处理

  1. temperaturemaintaining the temperature
  2. custombetween 30° and 40°
  3. temperatureAfter cooling
  4. customthe sodium sulfate and silver are separated from the reaction mixture by filtration
  5. customthe resulting filtrate is evaporated to dryness under vacuum
  6. customThe dry residue, after recrystallization
  7. additionfrom a mixture of benzene-hexane