반응 #1747869

반응 방정식

4-iodobenzoyl chloride

o-aminodiphenylamine

ammonia

→

N-Phenyl-2-(4-iodophenyl)benzimidazole

용매

ethanol

반응 조건

후처리

1. 1
   기타formed from 85-90° C
2. 2
   기타(5 min)
3. 3
   온도After cooling
4. 4
   여과The precipitate was filtered off with suction
5. 5
   세척washed with ethanol
6. 6
   workup.STIRRINGstirred up again in 400 ml of ethanol
7. 7
   기타which formed a solution which
8. 8
   온도After cooling to 5-10° C.
9. 9
   여과the precipitate was filtered off with suction
10. 10
    세척washed with cold ethanol
11. 11
    기타dried at 75° C. in a vacuum
12. 12
    기타drying cabinet
13. 13
    기타were obtained

실험 절차

37.47 g (136 mmol) of 97% 4-iodobenzoyl chloride and 12.82 g (68.2 mmol) of 98% o-aminodiphenylamine were heated to 100° C., in the course of which a stirrable melt formed from 85-90° C. Once the gas evolution had ended (5 min), the melt solidified. The reaction mixture was kept at 100° C. for another 3 hours. After cooling, it was admixed with 100 ml of ethanol with stirring. The precipitate was filtered off with suction, washed with ethanol and stirred up again in 400 ml of ethanol. The suspension was heated to 75° C., which formed a solution which was adjusted to pH 8 with 29 ml of 25% ammonia. After cooling to 5-10° C., the precipitate was filtered off with suction, washed with cold ethanol and dried at 75° C. in a vacuum drying cabinet. 18.37 g (68% of theory) of light gray microcrystals having an m.p. of 178-181° C. were obtained.

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