反应详情

To a stirred and cooled (0° C.) solution of 8.7 parts of N-[(4-fluorophenyl)methyl]-4-nitro-3-pyridinamine, 1-oxide and 150 parts of trichloromethane was added dropwise a solution of 10.2 parts of phosphor trichloride in 75 parts of trichloromethane. Upon completion, the mixture was allowed to reach room temperature and stirring was continued for one hour at reflux temperature. The reaction mixture was cooled and the solvent was evaporated. The residue was stirred intrichloromethane. The product was filtered off and dried, yielding 9 parts of N-[(4-fluorophenyl)methyl]-4-nitro-3-pyridinamine monohydrochloride (intermediate 13).

1. customto reach room temperature
2. stirringstirring
3. temperatureat reflux temperature
4. temperatureThe reaction mixture was cooled
5. customthe solvent was evaporated
6. stirringThe residue was stirred intrichloromethane
7. filtrationThe product was filtered off
8. customdried