反应详情

温度

27.5 °C

1-(3-Nitropropyl)-4-octylbenzene (37 g) and methanol (190 mL) are charged into a round bottom flask and stirred at 25-30° C. Paraformaldehyde (37 g) and triethylamine (38.52 g) are charged into the flask and the reaction mixture is heated to a reflux temperature (about 68° C.). The reaction mixture is maintained at the same temperature for about 2 hours and is cooled to a temperature of 25-30° C. The reaction mixture is evaporated under reduced pressure at a temperature of about 45° C. to obtain crude compound. Water (190 mL) and ethyl acetate (190 mL) are charged to the crude compound, stirred, and the organic layer is separated. The aqueous layer is extracted with ethyl acetate (190 mL) and the organic layer is combined with the initial organic layer. The combined organic layer is washed with water (190 mL) followed by brine solution (190 mL), dried over sodium sulphate, and evaporated under reduced pressure. Hexane (370 mL) is charged at 28° C. and the reaction mass is stirred at the same temperature for about 1 hour. The solid obtained is collected by filtration, washed with hexane (37 mL), and dried at 28° C. for about 3 hours to give 20.5 g of the title compound.

1. temperaturethe reaction mixture is heated to a reflux temperature (about 68° C.)
2. temperatureThe reaction mixture is maintained at the same temperature for about 2 hours
3. temperatureis cooled to a temperature of 25-30° C
4. customThe reaction mixture is evaporated under reduced pressure at a temperature of about 45° C.
5. customto obtain crude compound
6. stirringstirred
7. customthe organic layer is separated
8. extractionThe aqueous layer is extracted with ethyl acetate (190 mL)
9. washThe combined organic layer is washed with water (190 mL)
10. dry with materialdried over sodium sulphate
11. customevaporated under reduced pressure
12. additionHexane (370 mL) is charged at 28° C.
13. stirringthe reaction mass is stirred at the same temperature for about 1 hour
14. customThe solid obtained
15. filtrationis collected by filtration
16. washwashed with hexane (37 mL)
17. customdried at 28° C. for about 3 hours