Reaktion #1177527

Reaktionsgleichung

NaHCO3

PPSE

4,4'-dibromodiphenic acid

o-phenylene diamine

→

white crystals

Ausbeute 53.9%

4,4'-dibromo-2,2'-bisbenzimidazolyl biphenyl

Ausbeute 53.9%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturmaintained there for 20 hours
2. 2
   TemperaturThe solution was cooled
3. 3
   FiltrationThe product was filtered
4. 4
   Waschenwashed with 300 ml of hot methylene chloride
5. 5
   Extraktionextracted
6. 6
   Sonstige10% NaHCO3 overnight
7. 7
   SonstigeThe product was dried
8. 8
   Sonstigethen recrystallized from ethanol

Vorschrift

To the PPSE solution was added 15.0 g of 4,4'-dibromodiphenic acid, 8.11 g of o-phenylene diamine (recrystallized from methylene chloride and charcoal). This mixture was rapidly heated to 160° C. and maintained there for 20 hours. The solution was cooled, then poured into 2 1 of 10% NaHCO3 solution. The product was filtered, washed with 300 ml of hot methylene chloride, then extracted using a Soxhlet extractor using 10% NaHCO3 overnight. The product was dried then recrystallized from ethanol to give 11 g of white crystals, mp 326° C.-328° C. Analysis calculated for C26H16N4Br2 : C, 57.38; H, 2.96; N, 10.29. Found: C, 57.81; H, 3.04, N, 10.30.

Quelle