反应详情

温度

50 °C

2,3-Dimethoxy-6-nitrobenzaldehyde (40.0 g, 0.19 mole) was treated with acetone (275 mL) and warmed to 50° C. A solution of potassium permanganate in water (60 g/L) was added slowly at 50°-70° C. over a period of 16-20 hours until thin layer chromatographic analysis revealed complete absence of the starting material. Isopropanol (7.5 mL) was then added and the mixture was heated an additional hour. The precipitated manganese dioxide was removed by filtration and the filter cake was washed with 3% aqueous potassium hydroxide (ca 175-200 mL). The combined filtrates were acidified with hydrochloric acid and the precipitate was collected by filtration and dried in vacuo. The crude product was recrystallized from acetone to give the pure material, 28.3 g (67%), mp 187°-189° C.).

1. temperaturethe mixture was heated an additional hour
2. customThe precipitated manganese dioxide was removed by filtration
3. washthe filter cake was washed with 3% aqueous potassium hydroxide (ca 175-200 mL)
4. filtrationthe precipitate was collected by filtration
5. customdried in vacuo
6. customThe crude product was recrystallized from acetone
7. customto give the pure material, 28.3 g (67%), mp 187°-189° C.)