반응 #82977

반응 방정식

trichloroacetyl chloride

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

→

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

용매

xylene

반응 조건

후처리

1. 1
   기타obtained
2. 2
   온도The mixture is then heated
3. 3
   온도at reflux for two hours until the product which
4. 4
   기타has initially precipitated
5. 5
   workup.DISSOLUTIONis completely dissolved
6. 6
   온도Cool
7. 7
   여과filter
8. 8
   농축Concentrate the mother liquors
9. 9
   workup.ADDITIONadd petroleum ether
10. 10
    기타Combine with the precipitate obtained earlier
11. 11
    기타The combined precipitates
12. 12
    workup.ADDITIONare treated with an aqueous solution of sodium hydrogen carbonate
13. 13
    기타recrystallised from ethyl acetate

실험 절차

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.

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