HRID40413

反应详情

EQUATION

反应方程式

HRID 40413 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

13,13-dimethyl-6H-indeno[1,2-b]anthracene-6,11(13H)-dione (19 g, 0.058 mol) was dissolved in acetic acid (200 ml) and 57% HI (50 ml) was added thereto. The reaction mixture was stirred under reflux for 48 hours. After the reaction was terminated, the reaction solution was added with distilled water (500 ml). Then, the resultant solid was filtered and dissolved in toluene (200 ml), and iodine (4.56 g, 0.018 mol) was added thereto. The reaction mixture was stirred under reflux for 3 hours. After the reaction was terminated, the reaction solution was extracted and purified by column chromatography to give 13,13-dimethyl-13H-indeno[1,2-b]anthracene (10 g, yield=58%).

WORKUP

后处理

  1. temperatureunder reflux for 48 hours
  2. customAfter the reaction was terminated
  3. additionthe reaction solution was added with distilled water (500 ml)
  4. filtrationThen, the resultant solid was filtered
  5. dissolutiondissolved in toluene (200 ml)
  6. stirringThe reaction mixture was stirred
  7. temperatureunder reflux for 3 hours
  8. customAfter the reaction was terminated
  9. extractionthe reaction solution was extracted
  10. custompurified by column chromatography