反应详情

3,5-Dinitrobenzotrifluoride (10 g) was dissolved in a mixture of methanol (200 ml) and 1,4-dioxane (125 ml) and heated under reflux. To this solution was added concentrated hydrochloric acid (30 ml) and then in small portions, reduced iron powder (9 g). CARE: violent effervescence. Refluxing was continued for a further 1 hour and the reaction mixture allowed to cool to room temperature. The mixture was filtered through `Celite` and the pad washed well with dichloromethane. The solvents were removed under reduced pressure to give a residue which was partitioned between dichloromethane and water. The organic layer was washed with brine, dried (MgSO4) and evaporated under reduced pressure to give a brown semi-solid (8 g). This was chromatographed on silica gel using ethyl acetate-hexane (1:9) as eluant to give the title compound as fine golden crystals, yield 4.98 g.

1. temperatureheated
2. temperatureunder reflux
3. temperatureRefluxing
4. filtrationThe mixture was filtered through `Celite` and the pad
5. washwashed well with dichloromethane
6. customThe solvents were removed under reduced pressure
7. customto give a residue which
8. customwas partitioned between dichloromethane and water
9. washThe organic layer was washed with brine
10. dry with materialdried (MgSO4)
11. customevaporated under reduced pressure