Reacción #82977

Ecuación de reacción

trichloroacetyl chloride

2,9-dimethylimidazo[1,2-a]benzimidazole

→

2,9-Dimethyl-3-trichloroacetylimidazo[1,2-a]benzimidazole

Disolventes

xylene

Condiciones de reacción

Tratamiento posterior

1. 1
   Otroobtained
2. 2
   TemperaturaThe mixture is then heated
3. 3
   Temperaturaat reflux for two hours until the product which
4. 4
   Otrohas initially precipitated
5. 5
   workup.DISSOLUTIONis completely dissolved
6. 6
   TemperaturaCool
7. 7
   Filtraciónfilter
8. 8
   ConcentraciónConcentrate the mother liquors
9. 9
   workup.ADDITIONadd petroleum ether
10. 10
    OtroCombine with the precipitate obtained earlier
11. 11
    OtroThe combined precipitates
12. 12
    workup.ADDITIONare treated with an aqueous solution of sodium hydrogen carbonate
13. 13
    Otrorecrystallised from ethyl acetate

Procedimiento

Pour 5.45 g (30 mmol) of freshly distilled trichloroacetyl chloride dropwise into a boiling solution of 2,9-dimethylimidazo[1,2-a]benzimidazole (3.7 g; 20 mmol)--obtained as described in Khim. Geterotsikl Soedin, 86, (7), 918-925--in 50 ml of xylene, with vigorous stirring, over a period of 20 to 30 minutes. The mixture is then heated at reflux for two hours until the product which has initially precipitated is completely dissolved. Cool and filter. Concentrate the mother liquors and add petroleum ether. Combine with the precipitate obtained earlier and repeat the operation. The combined precipitates are treated with an aqueous solution of sodium hydrogen carbonate and then recrystallised from ethyl acetate.

Fuente