反应详情

4-Bromophenylacetonitrile (5.0 g, 25.5 mmol), hydroxylamine hydrochloride (3.9 g, 56.1 mmol), and sodium bicarbonate (5.1 g, 61.2 mmol) were dissolved in MeOH (250 mL, 6.2 mol) and water (40 mL, 2 mol). The mixture was heated at reflux overnight, cooled, and then concentrated to ˜50 mL. The residue was dissolved in DCM, washed with water and saturated aqueous NaCl, dried over MgSO4, filtered and concentrated to yield 2-(4-bromophenyl)-N-hydroxyacetamidine (5.0 g).

1. temperatureThe mixture was heated
2. temperatureat reflux overnight
3. temperaturecooled
4. concentrationconcentrated to ˜50 mL
5. dissolutionThe residue was dissolved in DCM
6. washwashed with water and saturated aqueous NaCl
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated