反应详情

A solution of 5.9 g (0.02 mole) of the above prepared 4-(2-chloro-1,1,2-trifluoroethoxy)-2,5-dichlorobenzeneamine in 100 ml toluene was placed in a 500 ml 3-necked round bottom flask fitted with a mechanical stirrer, thermometer and reflux condenser and 5.5 g (0.03 mole) of 2,6-difluorobenzoyl isocyanate was added while stirring. The temperature rose from 23° to 34° C. in a few minutes. The mixture was heated under reflux while stirring for one hour giving a clear solution which was cooled in an ice water bath. The toluene was removed by evaporation in a rotary evaporator and 25 ml acetic acid and 5 ml water were added to the residue. The resulting mixture was heated to boiling, giving a clear solution, cooled in an ice water bath and suction filtered. The filter cake obtained was washed with a little cold aqueous acetic acid and dried at room temperature. Weight, 8.5 g of white solid. m.p. 177°-179° C. The structure was verified by NMR.

1. customwas placed in a 500 ml 3-necked round bottom flask
2. customfitted with a mechanical stirrer
3. temperaturethermometer and reflux condenser
4. waitThe temperature rose from 23° to 34° C. in a few minutes
5. temperatureThe mixture was heated
6. temperatureunder reflux
7. stirringwhile stirring for one hour
8. customgiving a clear solution which
9. temperaturewas cooled in an ice water bath
10. customThe toluene was removed by evaporation in a rotary evaporator and 25 ml acetic acid and 5 ml water
11. additionwere added to the residue
12. temperatureThe resulting mixture was heated
13. customgiving a clear solution
14. temperaturecooled in an ice water bath
15. filtrationsuction filtered
16. customThe filter cake obtained
17. washwas washed with a little cold aqueous acetic acid
18. customdried at room temperature