تفاعل #68691

معادلة التفاعل

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

HI

iodine

→

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

المردود 58.6%

المذيبات

acetic acid

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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%).

المصدر