HRID357502

反应详情

EQUATION

反应方程式

HRID 357502 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A one liter flask equipped with a thermometer, stirrer and condenser is charged with 40 grams 6,13-dihydroquinacridone, 250 ml methanol and 52.8 grams 50% aqueous sodium hydroxide. The mixture is stirred under a slow flow of nitrogen at 50°-55° C. for one hour generating 6,13-dihydroquinacridone di-sodium salt. 0.8 grams anthraquinone-2-sulfonic acid sodium salt are added and the mixture is heated to reflux temperature. 73.5 grams of an aqueous 16.9% hydrogen peroxide solution are added into the reaction mixture with a peristaltic pump at a rate of 0.4 ml/minute maintaining reflux under a slow nitrogen flow over 2 hours and 35 minutes. The resulting reddish suspension is further stirred for 4 hours at reflux then filtered. The presscake is washed with methanol followed by hot water then dried, yielding 38.9 grams red quinacridone.

WORKUP

后处理

  1. customA one liter flask equipped with a thermometer, stirrer and condenser
  2. temperaturethe mixture is heated
  3. temperatureto reflux temperature
  4. temperaturemaintaining
  5. temperaturereflux under a slow nitrogen flow over 2 hours
  6. custom35 minutes
  7. stirringThe resulting reddish suspension is further stirred for 4 hours
  8. temperatureat reflux
  9. filtrationthen filtered
  10. washThe presscake is washed with methanol
  11. customthen dried