HRID430817

反应详情

EQUATION

反应方程式

HRID 430817 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
37.5 °C

PROCEDURE

实验过程

A one liter flask equipped with a thermometer, stirrer and condenser was charged with 40 grams 6,13-dihydroquinacridone, 250 ml methanol, 52.8 grams 50% aqueous sodium hydroxide and 3.0 grams 50% aqueous benzyl tributyl ammonium chloride. The mixture was stirred under a slow flow of nitrogen at 30 to 45° C. for five minutes, heated to 50 to 55° C. and stirred at 50 to 55° C. for one hour. 0.8 grams of the pigment additive toluene sulfonic acid methyl quinacridone in accordance with the teachings in pending application Ser. No. 60/118,405, was added, followed by the addition of 0.5 grams anthraquinone mono sulfonic acid sodium salt as catalyst, and the reaction mixture was heated to reflux. 73 grams of an aqueous 17% hydrogen peroxide solution were added into the reaction mixture with a peristaltic pump at a setting of 0.3 ml/minute maintaining reflux under a slow nitrogen flow. The resulting reddish suspension was further stirred for 10 minutes at reflux then diluted with 100 ml cold water and filtered. The presscake was washed with 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. temperatureheated to 50 to 55° C.
  3. stirringstirred at 50 to 55° C. for one hour
  4. addition60/118,405, was added
  5. temperaturethe reaction mixture was heated to reflux
  6. temperaturemaintaining
  7. temperaturereflux under a slow nitrogen flow
  8. stirringThe resulting reddish suspension was further stirred for 10 minutes
  9. temperatureat reflux
  10. filtrationfiltered
  11. washThe presscake was washed with hot water
  12. customthen dried