反应详情

3-(3-bromo-2,5-dichlorophenoxy)-4-chlorobenzene-1,2-diamine (2.48 g, 6.47 mmol) in acetic acid (20 mL) was cooled to 15° C., after which sodium nitrite (0.446 g, 6.47 mmol) in water (6.47 mL) was added dropwise under N2. After 1.5 hours, the reaction mixture was diluted with EtOAc (200 mL), and the organic phase was separated and washed with water (3×75 mL). The organic phase was dried (MgSO4), filtered, concentrated and placed under vacuum to yield the title compound. LRMS (M+1)=393.4.

1. customthe organic phase was separated
2. washwashed with water (3×75 mL)
3. dry with materialThe organic phase was dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated