反応 #68691

反応方程式

13,13-dimethyl-6H-indeno[1,2-b]anthracene-6,11(13H)-dione

HI

iodine

→

13,13-dimethyl-13H-indeno[1,2-b]anthracene

収率 58.6%

溶媒

acetic acid

反応条件

後処理

1. 1
   温度under reflux for 48 hours
2. 2
   その他After the reaction was terminated
3. 3
   workup.ADDITIONthe reaction solution was added with distilled water (500 ml)
4. 4
   ろ過Then, the resultant solid was filtered
5. 5
   workup.DISSOLUTIONdissolved in toluene (200 ml)
6. 6
   workup.STIRRINGThe reaction mixture was stirred
7. 7
   温度under reflux for 3 hours
8. 8
   その他After the reaction was terminated
9. 9
   抽出the reaction solution was extracted
10. 10
    その他purified by column chromatography

実験手順

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%).

出典