反应详情

温度

65 °C

To a warm solution of 3-methyl-4-nitrobenzaldehyde (1.0 equiv.) in methanol was added hydroxylamine hydrochloride (2.0 equiv.) and the mixture was stirred at 65° C. for 2 hours. Methanol was evaporated and the residue was diluted with ethyl acetate. The organic layer was washed with water, brine, dried over Na2SO4, filtered and concentrated in vacuo. The residue was then recrystallized from ethyl acetate and petroleum ether 60-80, to provide the title compound as a creamish solid (81%); 1H NMR (300 MHz, CDCl3) δ: 2.62 (s, 3H), 7.54-7.56 (m, 2H), 7.89 (s, 1H), 7.98-8.01 (d, J=9.0 Hz, 1H), 8.14 (s, 1H); IR (KBr) 3375, 3207, 3087, 2994, 1607, 1585, 1506, 1384, 1319, 1161, 986, 841, 755 cm−1.

1. customMethanol was evaporated
2. additionthe residue was diluted with ethyl acetate
3. washThe organic layer was washed with water, brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue was then recrystallized from ethyl acetate and petroleum ether 60-80