반응 #68691

반응 방정식

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

HI

iodine

→

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

수율 58.6%

용매

acetic acid

반응 조건

후처리

1. 1
   온도under reflux for 48 hours
2. 2
   기타After the reaction was terminated
3. 3
   workup.ADDITIONthe reaction solution was added with distilled water (500 ml)
4. 4
   여과Then, the resultant solid was filtered
5. 5
   workup.DISSOLUTIONdissolved in toluene (200 ml)
6. 6
   workup.STIRRINGThe reaction mixture was stirred
7. 7
   온도under reflux for 3 hours
8. 8
   기타After the reaction was terminated
9. 9
   추출the reaction solution was extracted
10. 10
    기타purified by column chromatography

실험 절차

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%).

출처