Reaktion #997028

Reaktionsgleichung

dimethylsulfate

1′H-2,2′-bibenzimidazole

sodium hydroxide

dimethylsulfate

sodium hydroxide

dimethylsulfate

→

white solid

1-Methyl-1H,1′H-2,2′-bibenzimidazole

Lösungsmittel

N,N-dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was heated to 45 C under nitrogen for 16 hours
2. 2
   workup.STIRRINGthe mixture was stirred at 45 C for 24 hours
3. 3
   Temperaturcooled to 22 C
4. 4
   Sonstigequenched with 350 ml water
5. 5
   FiltrationThe off-white solid was filtered
6. 6
   Waschenwashed with water
7. 7
   workup.DISSOLUTIONAfter dissolving the product in 125 ml hot ethanol
8. 8
   workup.ADDITION44 ml water were added
9. 9
   Temperaturthe solution was cooled to 5 C
10. 10
    Filtrationfiltered
11. 11
    Waschenwashed with 50% ethanol
12. 12
    Sonstigedried

Vorschrift

To a flask were added 1.2 g 1H, 1′H-2,2′-bibenzimidazole, 0.45 g sodium hydroxide, 100 ml N,N-dimethylformamide and 1.4 g dimethylsulfate. The mixture was heated to 45 C under nitrogen for 16 hours and another 0.45 g sodium hydroxide and 2.8 g dimethylsulfate were added and the mixture was stirred at 45 C for 24 hours. Another 4.2 g of dimethylsulfate were added and the mixture was stirred at 45 C for 24 hours, then cooled to 22 C and quenched with 350 ml water. The off-white solid was filtered and washed with water. After dissolving the product in 125 ml hot ethanol, 44 ml water were added and the solution was cooled to 5 C, filtered, washed with 50% ethanol and dried leaving 0.5 g white solid.

Quelle