反应详情

温度

70 °C

1-(3-nitropropyl)-4-octylbenzene (43 g) and absolute ethanol (400 mL) are charged into a round bottom flask equipped with a condenser and calcium guard tube. Paraformaldehyde (43 g) and triethylamine (64.8 mL) are added. The mixture is heated to 70° C., stirred for 3 hours, and is concentrated under reduced pressure at 50° C. to obtain a solid. The solid is dissolved in ethyl acetate (300 mL), the solution is washed with cold water (2×200 mL), and the organic layer is dried over anhydrous sodium sulphate. The organic layer is concentrated under reduced pressure to obtain a yellow solid. Hexane (500 mL) is added and the mixture is cooled to −20° C. and stirred for 20 minutes. The formed solid is separated by filtration and washed with cold hexane (2×100 mL) to obtain the title compound as an off-white solid. Yield: 26 g.

1. customequipped with a condenser and calcium guard tube
2. concentrationis concentrated under reduced pressure at 50° C.
3. customto obtain a solid
4. washthe solution is washed with cold water (2×200 mL)
5. dry with materialthe organic layer is dried over anhydrous sodium sulphate
6. concentrationThe organic layer is concentrated under reduced pressure
7. customto obtain a yellow solid
8. temperaturethe mixture is cooled to −20° C.
9. stirringstirred for 20 minutes
10. customThe formed solid is separated by filtration
11. washwashed with cold hexane (2×100 mL)