反应详情

Zinc dust (4.52 g, 69.2 mmol) was added to a stirred solution of 2-(4-bromo-2-nitrophenoxy)-N,N-dimethylethanamine (4 g, 13.8 mmol), ammonium chloride (3.7 g, 69.2 mmol), THF/Water (40/40 mL) at RT. Reaction completed in 4 hours. The RM was filtered and the filtrate was concentrated. The residue was dissolved in ethyl acetate and washed with water, dried over sodium sulfate, concentrated to get the crude mass which was washed with hexanes to afford titled compound 1.85 g (51.67% yield) as solid. 1H NMR (DMSO-d6, 300 MHz): δ 6.74-6.70 (m, 2H), 6.59-6.56 (m, 1H), 4.99 (s, 2H), 3.97-3.93 (t, 2H), 2.59-2.56 (t, 2H), 2.18 (s, 6H). LCMS: m/z=260.8 (M+2).

1. customReaction
2. filtrationThe RM was filtered
3. concentrationthe filtrate was concentrated
4. dissolutionThe residue was dissolved in ethyl acetate
5. washwashed with water
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated
8. customto get the crude mass which
9. washwas washed with hexanes