反应详情

A mixture of 5-Bromo-N,N-bis-(4-methoxy-benzyl)-N′-methyl-2-nitro-benzene-1,3-diamine (170 mmol), NH4Cl (2038 mmol) and Zn (2034 mmol) in 1:1 MeOH/THF (1 L) was stirred at room temperature for 1 h. The mixture was cooled to 0° C. and HCOOH (20 mL) was added slowly. The mixture was allowed to reach room temperature and stirred for 1 h. The mixture was filtered and combined with another one obtained following the procedure described above. The resulting mixture was concentrated. The residue was dissolved in DCM. The organic mixture was washed (sat. NH4Cl), dried (Na2SO4) and concentrated to afford the desired product.

1. temperatureThe mixture was cooled to 0° C.
2. customto reach room temperature
3. stirringstirred for 1 h
4. filtrationThe mixture was filtered
5. customobtained
6. concentrationThe resulting mixture was concentrated
7. dissolutionThe residue was dissolved in DCM
8. washThe organic mixture was washed (sat. NH4Cl)
9. dry with materialdried (Na2SO4)
10. concentrationconcentrated