反应详情

A solution of 2-hydroxy-3-methylbenzaldehyde (18.6 g), hydroxylamine hydrochloride (14.2 g) and sodium formate (19.2 g) in formic acid (200 mL) was heated at reflux for 18 h, then cooled and partitioned between DEE/water. The organic layer was washed with water, saturated aqueous sodium bicarbonate and brine, then dried over sodium sulfate and concentrated in vacuo to afford a solid. Recrystallization from diethyl ether/petroleum ether afforded the title compound as colorless crystals (15.0 g).

1. temperatureat reflux for 18 h
2. temperaturecooled
3. custompartitioned between DEE/water
4. washThe organic layer was washed with water, saturated aqueous sodium bicarbonate and brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated in vacuo
7. customto afford a solid
8. customRecrystallization from diethyl ether/petroleum ether