Reaktion #737494

Reaktionsgleichung

HCl

DMF

indene

para-amino-iodo-benzene

→

4-amino-phenyl-indene

Lösungsmittel

triethylamine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder reflux for 10 h
2. 2
   SonstigeForming precipitate
3. 3
   Sonstigewas separated
4. 4
   Waschenwashed with dichloromethane
5. 5
   workup.ADDITIONThe resulting substance was treated with the mixture 50 ml of dichloromethane and 50 ml of 5% KOH in water
6. 6
   SonstigeOrganic layer was separated
7. 7
   Waschenwashed twice with water
8. 8
   Filtrationfiltered
9. 9
   Trocknendried over Na2SO4
10. 10
    SonstigeDichloromethane was removed
11. 11
    Sonstigethe residue was recrystallized from 20 ml of EtOH

Vorschrift

20 ml of DMF, 2.2 g (20 mmol) of indene, 4,4 g (20 mmol) of para-amino-iodo-benzene, 2 ml of triethylamine and 0,134 (0,6 mmol) of Pd(OAc)2 were stirred under reflux for 10 h. The resulting mixture was poured into 200 ml of 15% HCl. Forming precipitate was separated and washed with dichloromethane. The resulting substance was treated with the mixture 50 ml of dichloromethane and 50 ml of 5% KOH in water. Organic layer was separated, washed twice with water, filtered and dried over Na2SO4. Dichloromethane was removed and the residue was recrystallized from 20 ml of EtOH. The yeld of product was 70%.

Quelle