تفاعل #1747869

معادلة التفاعل

4-iodobenzoyl chloride

o-aminodiphenylamine

ammonia

→

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

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   أخرىformed from 85-90° C
2. 2
   أخرى(5 min)
3. 3
   درجة الحرارةAfter cooling
4. 4
   ترشيحThe precipitate was filtered off with suction
5. 5
   غسيلwashed with ethanol
6. 6
   workup.STIRRINGstirred up again in 400 ml of ethanol
7. 7
   أخرىwhich formed a solution which
8. 8
   درجة الحرارةAfter cooling to 5-10° C.
9. 9
   ترشيحthe precipitate was filtered off with suction
10. 10
    غسيلwashed with cold ethanol
11. 11
    أخرىdried at 75° C. in a vacuum
12. 12
    أخرىdrying cabinet
13. 13
    أخرىwere obtained

الإجراء التجريبي

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.

المصدر