反应详情

To a solution of crude 4-methoxy-3,5-dinitro-benzoic acid (D24) (4.43 g, 17.3 mmol, 1 equiv) in MeOH (60 ml) was added concentrated H2SO4 (4 ml). The resulting mixture was refluxed for 3 h, cooled to room temperature and concentrated in vacuo. The residue was partitioned between H2O and AcOEt. The two layers were separated and the organic phase was washed with saturated aqueous NaHCO3 solution, dried over MgSO4 and concentrated in vacuo. Purification by flash chromatography on silica gel (iso-hexane/AcOEt: 85/15) gave 4-methoxy-3,5-dinitro-benzoic acid methyl ester (D25) (2.84 g, 65%) as an off white solid.

1. temperatureThe resulting mixture was refluxed for 3 h
2. concentrationconcentrated in vacuo
3. customThe residue was partitioned between H2O and AcOEt
4. customThe two layers were separated
5. washthe organic phase was washed with saturated aqueous NaHCO3 solution
6. dry with materialdried over MgSO4
7. concentrationconcentrated in vacuo
8. customPurification by flash chromatography on silica gel (iso-hexane/AcOEt: 85/15)