反应详情

0.34 g (0.001 mol) of [3-bromo-5-(4-nitrophenylsulphanyl)-phenyl]-methylamine was dissolved in 10 ml of acetonitrile, treated with 1.52 ml (0.020 mol) of formaldehyde, 0.74 g (0.010 mol) of NaBH3CN and 1.76 ml of acetic acid and stirred at room temperature for 1 hr. Thereafter, the solvent was removed, the residue was partitioned in ethyl acetate/water and the organic phase was washed with sat. sodium chloride solution, dried over MgSO4, filtered and concentrated. The residue was chromatographed on silica gel with ethyl acetate/hexane 1:19. There was obtained 0.35 g (99%) of [3-bromo-5-(4-nitro-phenylsulphanyl)-phenyl]-dimethylamine as yellow crystals; m.p.: 102-104° C.

1. customThereafter, the solvent was removed
2. customthe residue was partitioned in ethyl acetate/water
3. washthe organic phase was washed with sat. sodium chloride solution
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was chromatographed on silica gel with ethyl acetate/hexane 1:19