反应 #1747869

反应方程式

4-iodobenzoyl chloride

o-aminodiphenylamine

ammonia

→

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

溶剂

ethanol

反应条件

后处理

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

实验过程

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.

来源