HRID40413
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureunder reflux for 48 hours
- customAfter the reaction was terminated
- additionthe reaction solution was added with distilled water (500 ml)
- filtrationThen, the resultant solid was filtered
- dissolutiondissolved in toluene (200 ml)
- stirringThe reaction mixture was stirred
- temperatureunder reflux for 3 hours
- customAfter the reaction was terminated
- extractionthe reaction solution was extracted
- custompurified by column chromatography