反应详情

温度

100 °C

To a stirred mixture of 23.5 parts of N-(4-fluorophenylmethyl)-1,2-benzenediamine and 14.4 parts of concentrated hydrochloric acid were added dropwise 9 parts of cyanamide at 100° C. After stirring for 3 hours at 100° C., there were added dropwise 10.5 parts of a sodium hydroxide solution 50%. Upon completion, stirring was continued overnight at reflux temperature. The reaction mixture was cooled and taken up in a mixture of water, trichloromethane and N,N-dimethylformamide. The organic phase was separated, dried, filtered and evaporated. The residue was stirred in trichloromethane. The product was filtered off and crystallized from trichloromethane, yielding 2.5 parts (9.5%) of 1-(4-fluorophenylmethyl)-1H-benzimidazol-2-amine; mp. 189.5° C. (int. 31).

1. stirringUpon completion, stirring
2. waitwas continued overnight
3. temperatureat reflux temperature
4. temperatureThe reaction mixture was cooled
5. customThe organic phase was separated
6. customdried
7. filtrationfiltered
8. customevaporated
9. stirringThe residue was stirred in trichloromethane
10. filtrationThe product was filtered off
11. customcrystallized from trichloromethane