反应详情

To a stirred solution of di-methyl nitroterephthalate ((5), 12g, 50 mMol) in dioxane (100 mL) at room temperature was slowly added dropwise aq. 1N NaOH (50 mL) over 30 minutes. After stirring for 16 h at room temperature the reaction was diluted with water, washed with ether, acidified with aq. 1N HCl (50 mL) then extracted with 10% n-BuOH in ethyl acetate (2×100 mL). After drying (MgSO4) over ethyl acetate and evaporation under reduced pressure the resulting residue was purified by flash chromatography on silica gel eluted with (98:2:0.1) CHCl3, MeOH, HOAc to give product (6) (8.07 g, 72%) as a white solid.

1. washwashed with ether
2. extractionthen extracted with 10% n-BuOH in ethyl acetate (2×100 mL)
3. dry with materialAfter drying (MgSO4)
4. customover ethyl acetate and evaporation under reduced pressure the resulting residue
5. customwas purified by flash chromatography on silica gel
6. washeluted with (98:2:0.1) CHCl3, MeOH, HOAc