反应详情

To an ice cold solution of 3-bromo-5-nitro-benzoic acid (D5) (2.5 g, 10 mmol, 1 equiv) in MeOH (25 ml) was added SOCl2 (1 ml, 15 mmol, 1.5 equiv) dropwise. The resulting solution was allowed to warm to room temperature and was then stirred at 60° C. for 3 h, cooled to room temperature and concentrated in vacuo. The residue was dissolved in AcOEt and the organic layer was washed with saturated aqueous NaHCO3 solution, dried over MgSO4 and concentrated in vacuo to give 3-bromo-5-nitro-benzoic acid methyl ester (D11) (2.6 g, 100%) as a yellow solid. RT=3.22 min

1. temperaturecooled to room temperature
2. concentrationconcentrated in vacuo
3. dissolutionThe residue was dissolved in AcOEt
4. washthe organic layer was washed with saturated aqueous NaHCO3 solution
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo