反应详情

To a solution of 2,6-difluoro-3-methoxybenzonitrile (0.30 g, 1.70 mmol) in EtOH (10 ml) was added hydroxylamine hydrochloride (0.12 g, 1.70 mmol) and NaOH (0.071 g, 1.70 mmol). The resulting reaction mixture was refluxed for 15 h. After the completion of the reaction (TLC monitoring), the mixture was concentrated, added EtOH and filtered. The filtrate was evaporated in vacuo and the crude residue was purified over silica gel (60-120 M, 30% EtOAc-Hexane) to get the desired product (0.15 g, 42%) as a white solid.

1. customThe resulting reaction mixture
2. temperaturewas refluxed for 15 h
3. customAfter the completion of the reaction (TLC monitoring)
4. concentrationthe mixture was concentrated
5. additionadded EtOH
6. filtrationfiltered
7. customThe filtrate was evaporated in vacuo
8. customthe crude residue was purified over silica gel (60-120 M, 30% EtOAc-Hexane)