反応 #1747869

反応方程式

4-iodobenzoyl chloride

o-aminodiphenylamine

ammonia

→

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

溶媒

ethanol

反応条件

後処理

1. 1
   その他formed from 85-90° C
2. 2
   その他(5 min)
3. 3
   温度After cooling
4. 4
   ろ過The precipitate was filtered off with suction
5. 5
   洗浄washed with ethanol
6. 6
   workup.STIRRINGstirred up again in 400 ml of ethanol
7. 7
   その他which formed a solution which
8. 8
   温度After cooling to 5-10° C.
9. 9
   ろ過the precipitate was filtered off with suction
10. 10
    洗浄washed with cold ethanol
11. 11
    その他dried at 75° C. in a vacuum
12. 12
    その他drying cabinet
13. 13
    その他were obtained

実験手順

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.

出典