反应详情

100 g of O-trifluoromethylaniline is introduced at 20°±2° C. then 100 ml of dimethylacetamide is added while maintaining the same temperature. After cooling down under agitation at 0° C.±2° C. a solution of 88.8 g of dibromodimethylhydantoin and 100 ml of dimethylacetamide is then added over about 30 minutes while maintaining the temperature at 0° C.±2° C. The reaction medium is maintained under agitation for 30 minutes, then taken to 20° C.±2° C. and 40 g of dimethylhydantoin then 50 g copper oxide are added. The whole is heated under reflux for approximately 18 hours then cooled down to 20° C.±2° C., agitation is carried out for 30 minutes followed by filtering, separating and washing with 4×25 ml of dimethylacetamide. The resultant product is then poured into 300 ml of pure 22°Be ammonium hydroxide and 300 ml of demineralized water under agitation over 1 hour at 20° C.±2° C., agitation is continued for 1 hour at 20° C.±2° C. then the whole is cooled down to 0° C.±5° C. and is maintained under agitation for another hour, followed by separating, washing at 20° C.±2° C., with 100 ml of pure 22°Be ammonium hydroxide then with 4×100 ml of demineralized water and drying. In this way 155.8 g of expected product is obtained.

1. temperaturewhile maintaining the same temperature
2. additionis then added over about 30 minutes
3. temperaturewhile maintaining the temperature at 0° C.±2° C
4. temperatureThe reaction medium is maintained under agitation for 30 minutes
5. customtaken to 20° C.±2° C.
6. temperatureThe whole is heated
7. temperatureunder reflux for approximately 18 hours
8. temperaturethen cooled down to 20° C.±2° C.
9. filtrationby filtering
10. customseparating
11. washwashing with 4×25 ml of dimethylacetamide
12. additionThe resultant product is then poured into 300 ml of pure 22°Be ammonium hydroxide and 300 ml of demineralized water under agitation over 1 hour at 20° C.±2° C.
13. waitagitation is continued for 1 hour at 20° C.±2° C.
14. temperaturethe whole is cooled down to 0° C.±5° C.
15. temperatureis maintained under agitation for another hour
16. customby separating
17. washwashing at 20° C.±2° C., with 100 ml of pure 22°Be ammonium hydroxide
18. dry with materialwith 4×100 ml of demineralized water and drying